A small laser irradiation grafting and crosslinking system with controllable energy level and application method thereof

By integrating an adjustable laser source, a focusing optical system, and a real-time feedback control module, the problem of insufficient energy level control precision in material grafting and crosslinking technology is solved, achieving high-precision, low-energy-consumption, and environmentally friendly material processing, suitable for laboratory and field applications of various materials.

CN120002879BActive Publication Date: 2026-04-21HEILONGJIANG BINGLAN ZHICHUANG AEROSPACE TECHNOLOGY CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
HEILONGJIANG BINGLAN ZHICHUANG AEROSPACE TECHNOLOGY CO LTD
Filing Date
2025-03-31
Publication Date
2026-04-21

AI Technical Summary

Technical Problem

Existing material grafting and cross-linking technologies suffer from problems such as insufficient precision in energy level control, large equipment size, high environmental impact, and poor processing stability, making it difficult to meet the needs of small-batch processing in the laboratory and field applications.

Method used

By employing an adjustable laser source, focusing optical system, laser energy control module, processing platform, chemical reaction auxiliary module, and real-time monitoring and feedback system, combined with an intelligent control system, the laser energy can be precisely adjusted and the reaction environment can be dynamically controlled, ensuring processing accuracy and stability.

Benefits of technology

It achieves high-precision control of laser energy, significantly improves the controllability and processing quality of material grafting and cross-linking, reduces energy consumption, and enhances the flexibility and environmental friendliness of the equipment, making it suitable for the efficient processing of a variety of materials.

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Abstract

This invention relates to a small-scale laser irradiation grafting and crosslinking system with controllable energy levels and its application methods, belonging to the field of materials processing and modification technology. The system consists of an adjustable laser source, a focusing optical system, a laser energy control module, a processing platform, a chemical reaction auxiliary module, a real-time monitoring and feedback system, and an intelligent control system. It can precisely control the laser wavelength, power, and pulse width to achieve micron-level processing accuracy. Compared with traditional chemical grafting, thermally induced crosslinking, and plasma treatment methods, this invention has significant advantages such as non-contact processing, low energy consumption, high precision, and environmental friendliness. The system supports efficient grafting and crosslinking of various materials (such as polymers, metals, and ceramics), significantly improving processing efficiency and material properties, and providing innovative solutions for material functionalization and green manufacturing.
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Description

Technical Field

[0001] This invention belongs to the field of materials processing and modification technology, specifically relating to a small-scale laser irradiation grafting and crosslinking system with controllable energy levels and its application method. Background Technology

[0002] Material surface modification technology is widely used in polymer functional materials, biomedical devices, microelectronic devices, and other fields. Grafting or cross-linking methods can effectively improve the surface properties of materials, such as enhancing interfacial bonding, improving wear resistance and corrosion resistance, and introducing specific functional groups. Among these, grafting and cross-linking modification technologies have become important methods for functionalizing polymer materials. However, existing material grafting and cross-linking technologies still have many shortcomings.

[0003] Currently, commonly used surface grafting and crosslinking methods include chemical grafting, thermally induced crosslinking, plasma treatment, and laser irradiation. Chemical grafting typically relies on peroxide-based chemical initiators; while highly reactive, this often leads to polymer backbone degradation and residual byproducts, affecting material purity and performance stability. Thermally induced crosslinking, although a mature process, requires high temperatures, easily inducing thermo-oxidative aging and causing significant localized differences in crosslinking degree due to uneven temperature distribution, with common deviations reaching ±30%. Plasma treatment can achieve nanoscale surface modification, but the equipment consumes a lot of power, is complex to operate, and the modification effect is short-lived, typically less than 72 hours. Furthermore, while existing laser irradiation grafting and crosslinking technologies offer non-contact and precise processing, they still face the problem of insufficient laser energy level control precision, easily causing material ablation and uneven grafting, resulting in poor processing stability and insufficient product consistency.

[0004] Traditional grafting and cross-linking systems for materials are mostly bulky and have low system integration, making them difficult to meet the needs of small-batch processing in laboratories or field applications. These technologies generally have high energy consumption, heavy environmental impact, and insufficient green environmental protection, which limits their further application in the fine processing of high-performance materials.

[0005] In summary, existing material surface grafting and crosslinking technologies still face numerous bottlenecks in terms of controllability of reaction conditions, energy consumption management, equipment size, and adaptability. Therefore, there is an urgent need to develop a novel grafting and crosslinking system that features controllable energy levels, miniaturization, strong adaptability, and high processing precision to meet the demands for functionalization of polymer materials and efficient, environmentally friendly processing of various composite materials. Summary of the Invention

[0006] This invention addresses the problems of high material degradation risk, poor process controllability, and large environmental impact associated with traditional grafting and crosslinking technologies. It proposes a small-scale laser irradiation grafting and crosslinking system with controllable energy levels. The system achieves innovative breakthroughs through the following technical solutions:

[0007] The adjustable laser source uses a semiconductor laser with a wavelength range of 355nm to 1064nm, a power adjustment range of 0.1W to 10W, a pulse frequency of 1Hz to 1kHz, and is equipped with a built-in temperature control unit to ensure the stability and controllability of the laser output.

[0008] The focusing optical system includes an aspherical high-transmittance quartz lens and a gold-plated high-reflectivity mirror with a reflectivity greater than 99.5% and a reflection efficiency fluctuation of less than 0.5% within the incident angle range. The laser beam is efficiently transmitted and focused onto the surface of the material to be processed through the lens, mirror, and fiber optic transmission system. With the help of dynamic optical path adjustment function, multi-dimensional micro-displacement adjustment of the X / Y / Z axes can be achieved with a displacement accuracy of ±0.1μm, which can adapt to material surfaces of different thicknesses and morphologies and ensure processing accuracy.

[0009] The laser energy control module includes a beam splitter and a power control unit. It uses an electrically adjustable variable aperture and a polarizer to achieve fine adjustment of laser intensity. It can switch between single pulse, periodic pulse and continuous modes according to different material and process requirements. Combined with a real-time feedback system, it can dynamically adjust the laser output to achieve efficient and stable energy control.

[0010] The processing platform adopts a three-dimensional moving stage with high-precision positioning function, a moving accuracy of ±1μm, and a maximum stroke of 100mm×100mm×50mm. It supports automated processing of samples of different sizes and integrates a flexible fixing device and a vacuum adsorption system to ensure the stability of materials during processing and the precise execution of the processing path.

[0011] The chemical reaction auxiliary module includes a gas environment control system, which uses a mass flow meter to precisely regulate the flow rates of inert gases (nitrogen, argon) and active gases (oxygen). The nitrogen flow rate can be adjusted from 0.1 L / min to 10 L / min, and the oxygen flow rate can be adjusted from 0.05 L / min to 5 L / min. Combined with a gas mixing unit, it enables rapid switching and control of various atmospheric environments. The system has a real-time gas purity detection function to ensure the purity of the reaction environment. When the gas purity is lower than the set threshold, it automatically alarms and terminates the reaction process.

[0012] The real-time monitoring and feedback system includes a K-type thermocouple temperature sensor (measurement range -50℃ to 300℃, error ±0.5℃), a fiber optic spectrometer (wavelength resolution ±0.1nm, integration time 1ms to 1000ms), and a high-resolution CMOS camera (resolution 5MP, positioning error ±1μm). Through multi-sensor data fusion, it achieves comprehensive dynamic monitoring of the temperature, reaction process, and surface morphology of the processing area. Based on Kalman filtering and image edge detection algorithms, it provides real-time feedback and automatically corrects processing parameters, optimizing laser energy distribution and scanning path.

[0013] The intelligent control system adopts an embedded processor architecture, integrates operating software and human-machine interface, supports custom parameter settings, processing path planning, real-time data recording and full-process automated control, and has intelligent alarm and linkage protection functions for abnormal conditions, which significantly improves the convenience and safety of processing operations.

[0014] Furthermore, the power adjustment accuracy of the tunable laser source reaches 0.1mW, which can meet the diverse requirements of different materials and different reaction types for laser energy levels.

[0015] Furthermore, the focusing optical system is optimized through Zemax optical simulation to ensure that the diameter of the laser focusing spot is less than 5μm and the energy density distribution uniformity is better than 90%, making it suitable for submicron to nanoscale surface modification needs.

[0016] Furthermore, the dynamic optical path adjustment function is achieved through a piezoelectric ceramic micro-displacement platform, with synchronous adjustment of the X / Y / Z axes and a repeatability accuracy better than ±0.05μm, meeting the laser dynamic focusing requirements of materials with complex morphology.

[0017] Furthermore, the laser energy control module supports hierarchical energy scheduling to minimize material ablation and localized overheating during grafting or cross-linking.

[0018] Furthermore, the chemical reaction auxiliary module has a variety of preset typical process parameters and supports customized adjustment of the exclusive atmosphere environment for polypropylene, metals, ceramics and composite materials to meet diverse application scenarios.

[0019] Furthermore, the real-time monitoring and feedback system has a response time of less than 50ms, enabling sub-second automatic correction of laser parameters and ensuring high precision and consistency in the processing.

[0020] Furthermore, the intelligent control system has process optimization algorithms based on historical data and remote control interfaces, supports cloud storage of production data and multi-terminal synchronous management, and is suitable for various application scenarios such as laboratories, factories and field services.

[0021] The present invention also provides a laser irradiation grafting and crosslinking application method based on the above system, comprising the following steps:

[0022] (1) Material pretreatment: Deionized water and ultrasonic cleaning are used to clean the surface of the material to ensure that there are no impurities;

[0023] (2) Chemical solution preparation and coating: Maleic acid and photoinitiator are mixed in mass ratio and then sprayed evenly onto the surface of the material to be treated to form a reaction layer with a thickness of no more than 10 μm.

[0024] (3) Fixing and positioning: Fix the material on the sample stage through the processing platform to ensure that the surface is flat and within the laser irradiation focal point;

[0025] (4) Parameter setting and start processing: Set the laser wavelength (355nm to 1064nm), power (2W to 10W), pulse frequency (1Hz to 1kHz) and scanning speed (1mm / s to 10mm / s) according to the material properties;

[0026] (5) Irradiation treatment: Laser irradiation is carried out in a nitrogen-protected environment to ensure that the grafting or cross-linking reaction on the material surface is sufficient and uniform.

[0027] (6) Feedback optimization and real-time monitoring: Dynamically adjust laser parameters and scanning path based on real-time temperature and spectral data to avoid overheating or insufficient response;

[0028] (7) Post-processing and testing: After processing, the material is cleaned and dried, and the surface modification effect and mechanical property improvement are evaluated by SEM, FTIR, mechanical testing and other methods.

[0029] Based on the above technical solution, the energy-level controllable miniature laser irradiation grafting and crosslinking system of this invention, by integrating an adjustable laser source, a focusing optical system, and a dynamic energy regulation and real-time feedback control module, achieves high-precision and dynamic adjustment of laser energy, irradiation path, and reaction environment, significantly improving the controllability and processing quality of the material grafting and crosslinking process. This invention effectively solves the problems of coarse laser energy level regulation, lack of real-time feedback control in the processing process, large equipment size, and high environmental impact in existing technologies.

[0030] The miniaturized design of this invention makes the system suitable for various applications, including laboratory environments, small-scale production, and on-site processing, enhancing the flexibility and versatility of laser grafting and crosslinking technologies. Through its multi-wavelength, wide-power-range laser output capability, the system achieves compatible processing of various materials such as polymers, metals, and ceramics, providing an efficient solution for surface modification of different material systems.

[0031] Furthermore, the adoption of green and environmentally friendly processes avoids the chemical reagent residues and environmental pollution problems associated with traditional chemical methods. Laser processing consumes less energy, improving overall energy efficiency by over 30%, aligning with green manufacturing principles. Through intelligent control and automated management, this invention also significantly reduces operational barriers and reliance on manual labor, enhancing process stability and product consistency.

[0032] The present invention has the following advantages over the prior art:

[0033] 1. High Precision and High Efficiency: The laser energy offers strong controllability, and combined with a high-precision focusing optical system, it enables precise material modification at the micron or nanometer level, with processing areas as small as 1μm or less. Optimized laser pulse modes reduce processing speed, significantly shortening grafting and cross-linking times, resulting in efficiency improvements of over 50% compared to traditional chemical methods. A three-dimensional moving platform and automatic path control ensure uniform laser distribution within the processing area, leading to highly consistent processing results.

[0034] 2. Miniaturization and Portability: This system adopts a modular and lightweight design, significantly reducing the overall size and weight of the equipment, making it suitable for use in laboratories, research institutions, and industrial settings. The equipment is easy to install, can be quickly deployed, supports mobile and portable applications, and meets the needs of various scenarios.

[0035] 3. Environmental friendliness and low cost: Non-contact laser processing avoids reliance on catalysts, solvents, and other chemical reagents found in traditional chemical reactions, reducing environmental pollution and waste disposal costs. The laser source boasts high energy utilization and low power requirements, resulting in an overall energy consumption reduction of over 30%, aligning with green manufacturing principles.

[0036] 4. Multi-material compatibility: The system can precisely process polymers (such as PP, PVDF, etc.), composite materials, metals, and flexible electronic materials, adapting to the physical and chemical properties of different materials. The adjustable design of laser wavelength, power, and pulse width allows it to meet the grafting and cross-linking needs of various materials, making it extremely versatile.

[0037] 5. Intelligent and Automated: The system monitors the processing status in real time through temperature sensors, a spectral analysis module, and a high-definition camera, and dynamically optimizes laser parameters based on feedback to ensure processing quality. The intelligent control system automates the entire process from parameter setting and processing path planning to data recording, significantly reducing manual intervention and improving ease of operation.

[0038] 6. Significantly Improved Material Properties: Laser-induced chemical reactions are highly efficient, and the degree of grafting and cross-linking is controllable, significantly improving the mechanical strength, heat resistance, chemical resistance, and other properties of the material. By adjusting the laser parameters, various grafting and cross-linking effects can be achieved, meeting the diverse needs of materials in polymer composites, electronic devices, and biomedical materials.

[0039] 7. Wide range of applications: Suitable for small-batch sample preparation and performance testing in materials science, chemical engineering, and biomedicine. It has significant application value in precision manufacturing, flexible electronics, functional coatings, and high-performance composite material production. Its portable design allows for on-site material surface repair or functionalization in industrial settings.

[0040] In summary, this invention provides a high-precision, low-energy-consumption, environmentally friendly, and highly adaptable small-scale laser irradiation grafting and crosslinking system with controllable energy levels and its application method. It provides a new technical path for polymer surface modification, high-performance composite material preparation, and precision device manufacturing, and has significant application prospects and promotional value. Attached Figure Description

[0041] Figure 1 This is a block diagram of the overall system device of the present invention;

[0042] Figure 2 This is a schematic diagram of the irradiation system structure of the present invention;

[0043] Figure 3 This is a schematic diagram of the laser irradiator of the present invention;

[0044] Figure 4 This is a design diagram of the laser irradiator interface of the present invention;

[0045] Figure 5 This is a diagram showing the energy wave distribution generated by the laser irradiator of the present invention.

[0046] Figure 6 These are the optical lens morphology characterization and optical test diagrams of the present invention. Detailed Implementation

[0047] This invention relates to a small-scale laser irradiation grafting and crosslinking system with controllable energy levels, aiming to achieve high-precision and high-efficiency modification of material surfaces through laser irradiation technology. The specific embodiments of this invention are described in detail below with reference to the accompanying drawings and tables.

[0048] I. Example:

[0049] (1) System composition and working principle

[0050] The system of this invention mainly includes an adjustable laser source, a focusing optical system, a laser energy control module, a processing platform, a chemical reaction auxiliary module, a real-time monitoring and feedback system, and an intelligent control system. For example... Figure 1 As shown, the system achieves fully automated control of the laser irradiation grafting and crosslinking process through modular design.

[0051] 1. Adjustable laser source

[0052] The system uses a wide-wavelength semiconductor laser as the laser source, covering the 355nm to 1064nm band, with a power adjustment range of 0.1W to 10W and a pulse frequency of 1Hz to 1kHz. The laser has a built-in high-precision temperature control unit to maintain the laser cavity in the optimal operating state through temperature control, ensuring the stability of laser wavelength and power output.

[0053] The laser beam is guided into the focusing optical system via optical fiber or free-space transmission to ensure the stability and energy consistency of the laser output path. To achieve effective integration of the system with external control equipment, power supply systems, and safety interlocking mechanisms, the laser irradiator is equipped with various standardized interfaces (such as...). Figure 4 As shown, it includes a remote interlock socket, a USB socket, a universal input / output port, and a power voltage socket.

[0054] like Figure 3 The diagram shown illustrates the laser irradiator of this invention, illustrating the overall structural layout of the laser source and the detailed location of each functional interface. This interface design enables remote monitoring, data communication, laser start / stop control, and equipment operating status feedback, improving the ease of operation and system integration.

[0055] In addition, the technical parameters of the laser irradiator in this system are shown in Table 1:

[0056] Table 1 Technical parameters of laser irradiators

[0057]

[0058] Note: SM represents single-mode fiber, PM represents polarization-maintaining fiber, and MM represents multimode fiber. The system allows for flexible configuration of the fiber output mode according to processing requirements. Different wavelength and power configurations can flexibly meet the processing needs of various materials such as polymers, metals, and ceramics. Digital modulation up to 150MHz is compatible with high-speed modulation processes and enhances pulsed laser control capabilities.

[0059] 2. Focusing optical system

[0060] The focusing optical system uses an aspherical high-transmittance quartz lens (focal length 50mm, numerical aperture NA=0.6) and a gold-plated high-reflectivity mirror (reflectivity>99.5%) to focus the laser beam onto the surface of the material to be treated through the lens, mirror and fiber optic transmission system.

[0061] The system employs high-transmittance lens groups and mirrors with anti-reflective coatings, single-lens transmittance >99.8%, and overall optical path efficiency >95%, minimizing light loss. Dynamic optical path adjustment is achieved through a piezoelectric ceramic-driven micro-displacement platform, with X / Y / Z axis displacement accuracy of ±0.1μm and repeatability of ±0.05μm, supporting real-time calibration of focus position offset. The optical path calibration algorithm is based on CCD image feedback, automatically correcting optical path deviations through a Gaussian spot centroid positioning method (positioning error ±0.5μm). The adjustable focal length lens has a zoom range of ±10mm, driven by a stepper motor with a step size accuracy of 0.1μm, supporting flexible processing of materials of varying thicknesses. The optical path design has been verified through Zemax optical simulation, achieving a focused spot diameter <5μm and energy density distribution uniformity >90%.

[0062] like Figure 6 As shown, optical lens morphology characterization and optical testing indicate that the focused spot diameter is <5μm and the energy density distribution uniformity is >90%. The dynamic optical path adjustment function is achieved through a piezoelectric ceramic-driven micro-displacement platform, with X / Y / Z axis displacement accuracy of ±0.1μm and repeatability of ±0.05μm, supporting real-time calibration of focused position offset.

[0063] 3. Laser energy control module

[0064] The laser energy control module includes a beam splitter and a power control unit, supporting single-pulse, periodic pulse, and continuous mode switching. The beam splitter separates the master beam and reference beam to ensure energy control accuracy. The power control unit adjusts the laser intensity via electrically adjustable variable apertures, polarizers, etc. Figure 5 As shown, the energy waves generated by the laser irradiator can achieve multi-level processing through dynamic energy regulation.

[0065] 4. Processing platform

[0066] The machining platform is a three-dimensional moving stage with a movement accuracy of ±1μm and a maximum stroke of 100mm×100mm×50mm, equipped with a high-precision positioning system. The platform is connected to a computer or control system to ensure movement along a predetermined path and speed. Figure 2 As shown in the diagram, the structural schematic of the irradiation system illustrates the collaborative working method between the processing platform and the laser beam.

[0067] 5. Chemical Reaction Auxiliary Module

[0068] The chemical reaction auxiliary module integrates a gas environment control system, using a high-precision mass flow meter to dynamically balance nitrogen (N2), oxygen (O2), or argon (Ar), ensuring precise and controllable gas composition in the reaction environment. The system is equipped with a gas purity detection module that monitors gas purity in real time. When the detected gas purity falls below a set threshold (e.g., 99.99%), an alarm is automatically triggered and the reaction terminated, ensuring the safety and reliability of the experiment. Furthermore, the system has preset gas modes for different materials, such as:

[0069] Polypropylene grafting: A pure nitrogen environment is used with a flow rate of 5 L / min to avoid oxygen interfering with the grafting reaction.

[0070] Metal surface oxidation: A mixture of oxygen and nitrogen is used with a flow rate ratio of O2 2 L / min + N2 3 L / min to optimize the oxidation reaction effect.

[0071] Ceramic activation: A pure argon gas environment is used with a flow rate of 8L / min to ensure efficient activation of the ceramic surface.

[0072] With flexible gas ratios and preset modes, the chemical reaction auxiliary module can meet the processing needs of various materials, significantly improving the accuracy and efficiency of the reaction.

[0073] The gas environment control system provides inert gas (such as nitrogen and argon) protection to prevent oxygen from interfering with the reaction. The system uses a mass flow meter for closed-loop feedback control. The nitrogen flow rate is adjustable from 0.1 to 10 L / min with a control accuracy of ±0.05 L / min; the oxygen flow rate is adjustable from 0.05 to 5 L / min with an accuracy of ±0.03 L / min. The system can introduce oxygen to promote certain oxidation reactions and achieves a dynamic N2 / O2 ratio through a gas mixing unit (e.g., nitrogen ≥95% in reduction reactions, oxygen 5-50% in oxidation reactions). For different materials, the system has preset gas modes: polypropylene grafting (N2 flow rate 5 L / min), metal surface oxidation (O2 flow rate 2 L / min + N2 3 L / min), and ceramic activation (Ar flow rate 8 L / min). Furthermore, the system has a built-in gas purity detection module (detection accuracy ±0.1%), which will automatically alarm and terminate the reaction when the gas purity is below 99.99%.

[0074] 6. Real-time monitoring and feedback system

[0075] The system includes a K-type thermocouple temperature sensor (measuring range -50 to 300℃, error ±0.5℃), a fiber optic spectrometer with a wavelength resolution of ±0.1nm and an integration time of 1-1000ms, and an image analysis module consisting of a CMOS camera (5MP resolution, positioning error ±1μm). This system is used to monitor the temperature, reaction state, and surface morphology of the processing area in real time, and dynamically optimize laser parameters. The data processing algorithm employs Kalman filtering (multi-sensor data fusion error <1%) and the Canny edge detection algorithm (pixel-level error ±0.5px), with a feedback response time of <50ms, enabling dynamic optimization of the processing.

[0076] 7. Intelligent Control System

[0077] The intelligent control system is based on an embedded processor and integrates a software interface, providing functions such as parameter setting, data recording, and automated control of the processing. The system monitors the processing status in real time through temperature sensors, a spectral analysis module, and a high-definition camera, and dynamically optimizes laser parameters based on feedback.

[0078] How this system works:

[0079] First, a laser beam suitable for the target material is emitted from a tunable laser source (with appropriate wavelength, power, and pulse width selected). The laser beam is precisely focused onto the material surface by a focusing optics system, forming a high-energy-density processing area. Second, under the high-energy irradiation of the laser, molecules on the material surface are excited. These excited molecules combine with reactants to form grafted structures, or cross-linked structures are formed through high-energy collisions. Next, the sample is moved along a pre-set trajectory by a processing platform, ensuring uniform laser processing within the designated area. Three-dimensional movement allows for multi-layered or complex-shaped grafting and cross-linking. Real-time monitoring and feedback adjustments are then implemented. A temperature sensor detects the temperature of the processing area to prevent overheating and material degradation. A spectral analysis module monitors the chemical reaction state in real time to ensure complete grafting and cross-linking. The system dynamically adjusts the laser power, pulse width, or path based on feedback data to guarantee processing accuracy and stability. Finally, after processing, the surface morphology and performance data recorded by the monitoring system are used for quality assessment. A complete data report of the processing process is generated for subsequent process optimization and mass production reference.

[0080] Based on the above composition and working principle, this invention realizes an efficient, precise, and environmentally friendly material grafting and cross-linking process, which is applicable to a variety of application scenarios and material types.

[0081] II. Specific Application Examples

[0082] (1) Material preparation

[0083] 1. Polypropylene (PP) film: Select commercially available polypropylene film with a thickness of 0.1mm, cut to a size of 30mm×30mm suitable for experimental or production requirements.

[0084] 2. Maleic acid: Select maleic acid of appropriate specifications with a purity ≥99.5%.

[0085] 3. Photoinitiator: Ammonium persulfate (APS) should be selected, with a purity of ≥98%.

[0086] 4. Deionized water: used to dissolve maleic acid and photosensitizer.

[0087] 5. Sample pretreatment: Dissolve 10g of maleic acid in 90mL of deionized water to prepare a 10wt.% maleic acid solution. Add ammonium persulfate photoinitiator (concentration of 1% of the mass of maleic acid) and stir thoroughly until completely dissolved.

[0088] 6. Sample Fixation and Installation: Fix the material sample on the processing platform to ensure that the sample remains stable and does not move during laser irradiation. Fixation methods include using mechanical clamps or suction cups.

[0089] 7. Optical testing of materials: Before laser processing, a spectrometer is used to test the transmittance of the materials and select materials suitable for the laser wavelength to improve the absorption efficiency of laser energy.

[0090] (2) Equipment connection and debugging

[0091] 1. The output of the laser needs to be connected to a focusing optical system (such as a lens, mirror, etc.) via an adapter to ensure that the laser beam is accurately transmitted to the material to be processed.

[0092] 2. The laser beam is transmitted to the focusing lens via optical fiber or free space. Ensure the optical fiber connection is secure and adjust the insertion angle of the fiber to ensure the laser beam travels along the correct path.

[0093] 3. The 3D platform needs to be connected to a computer or control system to ensure it can move along the predetermined path and speed. Connect the platform's drive motor, power supply, and sensor system to ensure the platform's movement accuracy and stability. Connect the temperature control platform and adjust its temperature range and control accuracy to ensure the sample temperature remains stable near the set value during processing.

[0094] 4. Install a high-definition or infrared camera to monitor the sample surface condition in real time during laser processing. Image processing software is used to acquire real-time information about the sample surface reaction, ensuring uniformity and consistency of the processing. A CCD camera acquires focused spot images, and a centroid positioning algorithm is used to calculate the spot offset, driving the piezoelectric ceramic platform to compensate for positional deviations within ±0.5μm.

[0095] 5. Before starting the laser, set the target temperature to 25℃ using the PID control algorithm. After the temperature control unit stabilizes within the ±0.1℃ range, perform laser output calibration.

[0096] 6. Set up a feedback mechanism for parameters such as temperature and power. When the system detects abnormal processing conditions, it will automatically adjust the laser parameters or processing path to ensure that the processing is always in the best condition.

[0097] (3) Experimental Operation

[0098] 1. Place the cleaned PP sample on the experimental platform, ensuring that the sample is fixed and in the laser irradiation area.

[0099] 2. Using a micro-spraying system, uniformly coat the maleic acid solution onto the PP film surface, ensuring complete coverage of the sample surface and avoiding any missed areas. Control the coating thickness to within 10 μm. After coating, allow it to stand for 10 minutes to ensure the solution forms a uniform film on the PP surface.

[0100] 3. Start the laser and the laser system. Set the laser power to 5W, wavelength to 355nm (matching the absorption peak of maleic anhydride), pulse frequency to 50Hz, and pulse width to 10ns-1ms.

[0101] 4. Under nitrogen protection (flow rate 5 L / min, purity 99.99%), the sample surface was laser scanned at a scanning speed of 5 mm / s for 3 minutes.

[0102] 5. When the laser beam irradiates, the three-dimensional platform will move smoothly according to the set path and speed, so that the laser beam will evenly irradiate the surface of the PP sample.

[0103] 6. After laser irradiation, gently wipe the sample with deionized water to remove unreacted maleic acid and initiator residue.

[0104] 7. Place the sample in a vacuum drying oven, set the temperature to 40℃, and dry for 30 minutes.

[0105] (4) Performance evaluation

[0106] 1. Observe the surface morphology of PP samples after laser irradiation using scanning electron microscopy (SEM). Analyze the changes in the microstructure of the PP sample surface to determine whether the grafting reaction was successful.

[0107] 2. Compare the surface morphology before and after the treatment to see if any new structures have been formed or if there are any changes in surface roughness.

[0108] 3. Use Fourier transform infrared spectroscopy (FTIR) to analyze the chemical changes on the sample surface. Compare the FTIR spectra before and after grafting, and observe whether characteristic MA peaks (such as absorption peaks of functional groups like C=O and C=C) appear, thereby verifying the occurrence of the grafting reaction.

[0109] 4. Evaluate the mechanical properties of the grafted PP samples using methods such as tensile testing and hardness testing. Grafting typically improves the surface strength, abrasion resistance, and tensile strength of the material.

[0110] 5. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to test the thermal stability of the samples. Grafting reaction can improve the thermal stability of PP. During the test, the thermal degradation temperature and thermal decomposition characteristics of the samples were analyzed.

[0111] 6. Use solubility testing (e.g., dissolving in a suitable solvent) or other quantitative methods to determine the grafting degree and verify the effect of grafting MA onto PP under laser irradiation.

[0112] III. Experimental Results and Data Analysis

[0113] Based on the experimental data, Table 2 shows a comparison of the experimental results of the system of the present invention with those of traditional chemical methods:

[0114] Table 2 Comparative Experimental Data Table

[0115] index Traditional chemical method This invention Increase Grafting rate (%) 65±5 88±3 35% Reaction time (min) 120 8 93% Energy consumption (kWh / kg) 2.5 0.3 88%

[0116] According to the comparative experimental data in Table 2, the grafting rate of this invention is 88±3%, which is 35% higher than that of the traditional chemical method (65±5%). The reaction time is shortened from 120 minutes to 8 minutes, and the efficiency is improved by 93%. Energy consumption is reduced from 2.5 kWh / kg to 0.3 kWh / kg, a reduction of 88%.

[0117] IV. Optimization Range of Process Parameters for Different Materials

[0118] The system has set specific process parameters for different types of materials, as shown in Table 3:

[0119] Table 3 shows the optimization range of process parameters for different materials.

[0120]

[0121] As shown in Table 3, the optimized range of process parameters for different materials indicates that this system can meet the grafting and crosslinking requirements of polymers, metals, composite materials and ceramics, and has extremely strong applicability.

[0122] By integrating the experimental data and process parameter optimization results from Tables 2 and 3, the energy-level controllable miniature laser irradiation grafting and crosslinking system of this invention demonstrates significant process advantages in various material application fields. The system employs a miniaturized design, combined with low energy consumption and high-precision control, enabling efficient surface modification and functionalization development of high-performance products such as polymer composites, electronic devices, and medical materials. Compared to traditional processes, this system achieves significant improvements in grafting rate, reaction time, and energy consumption. For example, the grafting rate increases from 65±5% in traditional chemical methods to 88±3%, the reaction time is shortened from 120 minutes to 8 minutes, and energy consumption is reduced from 2.5 kWh / kg to 0.3 kWh / kg. Furthermore, the system utilizes a green and environmentally friendly process, significantly reducing energy consumption and pollution risks during grafting and crosslinking, providing an innovative solution for achieving green material manufacturing.

[0123] This invention successfully solves multiple technical challenges of traditional grafting and crosslinking technologies, including reaction control, environmental adaptability, efficiency, material compatibility, processing precision, and equipment size, through a small-scale laser irradiation grafting and crosslinking system with controllable energy levels. Through precise energy control, modular design, and intelligent feedback mechanisms, the system significantly improves the efficiency, precision, and environmental friendliness of material grafting and crosslinking processes. For example, the system supports the processing of various materials, such as polymers (PP, PVDF, etc.), metals (stainless steel), composite materials (CFRP), and ceramics (Al2O3), and achieves high-precision processing through dynamic parameter control, with processing areas as small as less than 1 μm. This system provides a green, efficient, and precise solution for the functionalization of polymer materials and the development of high-performance composite materials, promoting the development of material modification technology towards a more intelligent and environmentally friendly direction.

Claims

1. A small-scale laser irradiation grafting and cross-linking system with controllable energy levels, characterized in that, include: An adjustable laser source, wherein the laser source is a semiconductor laser with a wavelength range of 355nm to 1064nm, a power adjustment range of 0.1W to 10W, a pulse frequency of 1Hz to 1kHz, a control capability with a power adjustment accuracy of 0.1mW, and is equipped with a built-in temperature control unit. The focusing optical system includes an aspherical quartz lens and a gold-plated high-reflectivity mirror. The lens has a focal length of 50 mm and a numerical aperture of 0.

6. The laser beam is focused onto the surface of the material to be treated through the lens, mirror, and fiber optic transmission system. It has a dynamic optical path adjustment function achieved by a three-axis micro-displacement platform driven by piezoelectric ceramics, with a displacement accuracy of ±0.1 μm and a repeatability of ±0.05 μm. The laser energy control module includes a beam splitter and a power control unit, supporting switching between single-pulse, periodic pulse, and continuous modes; The processing platform is a three-dimensional moving stage with a moving accuracy of ±1μm and a maximum stroke of 100mm×100mm×50mm. It is used to carry the material to be processed and to perform dynamic scanning in conjunction with the processing path. The chemical reaction auxiliary module includes a gas environment control system, which uses a mass flow meter to dynamically adjust the flow rate of nitrogen, oxygen or argon. The nitrogen flow rate can be adjusted from 0.1 L / min to 10 L / min, and the oxygen flow rate can be adjusted from 0.05 L / min to 5 L / min. It also has gas purity detection and alarm functions. The real-time monitoring and feedback system includes a K-type thermocouple temperature sensor, a fiber optic spectrometer with a wavelength resolution of ±0.1nm and an integration time of 1ms to 1000ms, and an image analysis module with a resolution of 5MP and a positioning error of ±1μm, used to monitor the temperature, reaction state and surface morphology of the processing area in real time. The intelligent control system, based on an embedded processor and integrating a software interface, has the functions of parameter setting, data recording, and automatic control of the processing process. It has an automatic alarm mechanism that automatically stops processing when the gas purity is detected to be lower than 99.99% or when the system is abnormal.

2. The system according to claim 1, characterized in that, The optical path calibration algorithm is based on CCD image feedback and uses the Gaussian spot centroid positioning method to automatically correct optical path deviations, with a positioning error of ±0.5μm.

3. The system according to claim 1, characterized in that, The image analysis module uses a CMOS image sensor.

4. The system according to claim 1, characterized in that, The intelligent control system further includes a process optimization algorithm module.

5. The system according to claim 1, characterized in that, The chemical reaction auxiliary module has a multi-gas mixing function, which can automatically switch the gas combination mode according to the preset atmosphere requirements, and can be applied to different processing scenarios of polypropylene, metal or ceramic materials.

6. An application method based on the energy level controllable small-scale laser irradiation grafting and crosslinking system as described in any one of claims 1 to 5, characterized in that, Includes the following steps: S1. Material pretreatment: Coating the surface of the polypropylene film with a solution of maleic acid and photoinitiator. S2. Fix the material to be processed on the processing platform to ensure stability; S3. Start the laser system, set the laser wavelength, power and pulse frequency, and control the scanning speed; S4. Under a nitrogen-protected environment, material surface grafting or cross-linking is achieved through laser irradiation; S5. Through a real-time monitoring and feedback system, laser parameters are dynamically adjusted to ensure processing accuracy; S6. After irradiation, clean and dry the material, and perform surface performance testing and evaluation.

Citation Information

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