Energy-level-controllable small laser irradiation grafting and crosslinking system and application method thereof

Abstract

The invention relates to an energy-level-controllable small laser irradiation grafting and crosslinking system and an application method thereof, and belongs to the technical field of material processing and modification. The system is composed of an adjustable laser source, a focusing optical system, a laser energy regulation and control module, a machining platform, a chemical reaction auxiliary module, a real-time monitoring and feedback system and an intelligent control system, laser wavelength, power and pulse width can be accurately controlled, and micron-level machining precision is achieved. Compared with a traditional chemical grafting method, a thermal induction crosslinking method and a plasma treatment method, the method has the remarkable advantages of non-contact processing, low energy consumption, high precision, environmental friendliness and the like. The system supports efficient grafting and crosslinking of various materials (such as polymers, metals and ceramics), the processing efficiency and the material performance are remarkably improved, and an innovative solution is provided for material functionalization and green manufacturing.

Description

Technical Field

[0001] The invention belongs to the technical field of material processing and modification, and in particular relates to a small laser irradiation grafting and cross-linking system with controllable energy levels and an application method thereof. Background Art

[0002] Material surface modification technology is widely used in the fields of polymer functional materials, biomedical devices, microelectronic devices, etc. Grafting or cross-linking 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 them, grafting and cross-linking modification technology has become an important method for functionalizing polymer materials. However, the existing material grafting and cross-linking technology still has many shortcomings.

[0003] Currently, the commonly used surface grafting and cross-linking methods include chemical grafting, thermal induced cross-linking, plasma treatment and laser irradiation. Chemical grafting usually relies on peroxide chemical initiators. While having high reaction activity, it often leads to degradation of the polymer main chain, accompanied by residual by-products, affecting the purity and performance stability of the material. Although the thermal induced cross-linking method is mature, it needs to be carried out in a high temperature environment, which is easy to cause thermal oxidation aging of the material, and the local cross-linking degree varies greatly due to uneven temperature distribution, with common deviations up to ±30%. The plasma treatment method can achieve nanoscale modification of the material surface, but the equipment power consumption is high, the operation is complicated, and the modification effect is short-lived, usually less than 72 hours. In addition, although the existing laser irradiation grafting and cross-linking technology has the characteristics of non-contact and fine processing, it still faces the problem of insufficient precision in laser energy level regulation, which is easy to cause material ablation, uneven grafting and other phenomena, resulting in poor processing stability and insufficient product consistency.

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

[0005] In summary, the existing material surface grafting and cross-linking technology still has many bottlenecks in terms of controllability of reaction conditions, energy consumption management, equipment volume and adaptability. Therefore, it is urgent to develop a new grafting and cross-linking system with controllable energy levels, miniaturized systems, strong adaptability and high processing precision to meet the needs of functionalization of polymer materials and efficient and environmentally friendly processing of various composite materials. Summary of the invention

[0006] In view of the high risk of material degradation, poor process controllability, and high environmental load in traditional grafting and cross-linking technologies, this invention proposes a small laser irradiation grafting and cross-linking system with controllable energy levels. The system achieves innovative breakthroughs through the following technical solutions:

[0007] The adjustable laser source adopts 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] Focusing optical system, the focusing optical system includes a high-transmittance quartz lens with an aspherical design and a high-reflectivity reflector with gold-plated surface, the reflectivity is greater than 99.5%, and the fluctuation of reflection efficiency within the incident angle range is less than 0.5%. The laser beam is efficiently transmitted and focused to the surface of the material to be processed through the lens, the reflector and the optical fiber transmission system, and the dynamic optical path adjustment function is combined to realize multi-dimensional micro-displacement adjustment of the X / Y / Z axis, and the displacement accuracy reaches ±0.1μm, which is suitable for material surfaces of different thicknesses and morphologies to ensure processing accuracy;

[0009] Laser energy control module, which includes a beam splitter and a power control unit. It uses an electrically adjustable variable iris and a polarizer to achieve fine adjustment of laser intensity. It can select single pulse, periodic pulse and continuous mode switching according to different material and process requirements, and dynamically adjust the laser output in combination with a real-time feedback system to achieve efficient and stable energy control;

[0010] The processing platform adopts a three-dimensional moving table with high-precision positioning function, a moving accuracy of ±1μm, a maximum travel of 100mm×100mm×50mm, supports the automated processing of samples of different sizes, and integrates a flexible fixture and a vacuum adsorption system to ensure the stability of the material during processing and the precise execution of the processing path;

[0011] Chemical reaction auxiliary module, including gas environment control system, can realize precise regulation of inert gas (nitrogen, argon) and active gas (oxygen) flow through mass flow meter, with nitrogen flow regulation range of 0.1L / min to 10L / min, oxygen flow regulation range of 0.05L / min to 5L / min, combined with gas mixing unit to realize rapid switching and control of various atmosphere environments, the system has real-time gas purity detection function to ensure the purity of reaction environment, and automatically alarms and terminates the reaction process when gas purity is lower than the set threshold;

[0012] Real-time monitoring and feedback system, including K-type thermocouple temperature sensor (measuring range -50℃ to 300℃, error ±0.5℃), fiber spectrometer (wavelength resolution ±0.1nm, integration time 1ms to 1000ms) and high-resolution CMOS camera (resolution 5MP, positioning error ±1μm), through multi-sensor data fusion, to achieve all-round dynamic monitoring of processing area temperature, reaction progress and surface morphology, and based on Kalman filtering and image edge detection algorithm, real-time feedback and automatic correction of processing parameters, optimize laser energy distribution and scanning path;

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

[0014] Furthermore, the power adjustment accuracy of the adjustable laser source reaches 0.1 mW, 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 laser focusing spot diameter is less than 5μm and the energy density distribution uniformity is better than 90%, which is suitable for submicron to nanometer surface modification needs.

[0016] Furthermore, the dynamic optical path adjustment function is realized through a piezoelectric ceramic micro-displacement platform, with X / Y / Z three-axis synchronous adjustment and a repeated positioning accuracy better than ±0.05μm, which can meet the laser dynamic focusing requirements of materials with complex morphology.

[0017] Furthermore, the laser energy regulation module supports graded energy scheduling to minimize material ablation and local overheating problems during the grafting or cross-linking process.

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

[0019] Furthermore, the response time of the real-time monitoring and feedback system is less than 50ms, which can achieve sub-second automatic correction of laser parameters and ensure high precision and consistency of the processing process.

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

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

[0022] (1) Material pretreatment: Use deionized water and ultrasonic cleaning to clean the material surface to ensure that there is no impurity contamination;

[0023] (2) Chemical solution preparation and coating: maleic acid and photosensitive initiator are mixed according to the mass ratio and evenly sprayed on 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 focus of the laser irradiation;

[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 performed under a nitrogen protection 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 paths 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 small laser irradiation grafting and cross-linking system of the embodiment of the present invention realizes high-precision and dynamic adjustment of laser energy, irradiation path and reaction environment by integrating adjustable laser source, focusing optical system, dynamic energy regulation and real-time feedback control module, and significantly improves the controllability and processing quality of material grafting and cross-linking process. The present invention effectively solves the problems of extensive laser energy level regulation, lack of real-time feedback control in the processing process, large equipment volume and high environmental load in the prior art.

[0030] The miniaturized design of the present invention makes the system suitable for a variety of application scenarios such as laboratory environments, small-scale production and on-site processing, and improves the flexibility and universality of laser grafting and cross-linking technology. The system achieves compatibility processing of multiple types of materials such as polymers, metals, and ceramics through multi-wavelength and wide power range laser output capabilities, providing an efficient solution for surface modification of different material systems.

[0031] In addition, the green and environmentally friendly process is adopted to avoid the problems of chemical reagent residue and environmental pollution in traditional chemical methods. The laser processing process has low energy consumption and the overall energy efficiency ratio is improved by more than 30%, which is in line with the concept of green manufacturing. Through intelligent control and automated management, the present invention also significantly reduces the operating threshold and dependence on manual labor, and improves process stability and product consistency.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] 1. High precision and high efficiency: The laser energy is highly controllable, and combined with a high-precision focusing optical system, it can achieve precise material modification at the micron or nanometer level, and the minimum processing area can be less than 1μm. The laser pulse mode optimizes the processing rate, significantly shortens the grafting and cross-linking time, and improves the efficiency by more than 50% compared with traditional chemical methods. Through the three-dimensional mobile platform and automatic path control function, the laser distribution in the processing area is ensured to be uniform and the processing effect is highly consistent.

[0034] 2. Miniaturization and portability: This system adopts modular and lightweight design, and the overall equipment size and weight are greatly reduced, which is suitable for use in laboratories, scientific research and industrial sites. The equipment is easy to install and can be deployed quickly, supporting mobile and portable applications to meet the needs of multiple scenarios.

[0035] 3. Environmental protection and low cost: Through non-contact laser processing technology, the dependence on catalysts, solvents and other chemical reagents in traditional chemical reactions is avoided, reducing environmental pollution and waste disposal costs. The laser source has high energy utilization, low power demand, and overall energy consumption is reduced by more than 30%, which is in line with the concept of green manufacturing.

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

[0037] 5. Intelligence and automation: The processing status is monitored in real time through temperature sensors, spectrum analysis modules and high-definition cameras, and laser parameters are dynamically optimized based on feedback to ensure processing quality. The intelligent control system realizes full process automation from parameter setting, processing path planning to data recording, greatly reducing manual intervention and improving operational convenience.

[0038] 6. Significant improvement in material performance: 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, a variety of grafting and cross-linking effects can be achieved to meet the diverse needs of materials in polymer composites, electronic devices and biomedical materials.

[0039] 7. Wide application scenarios: Suitable for small batch sample preparation and performance testing in the fields of material science, chemical engineering and biomedicine. It has important application value in precision manufacturing, flexible electronics, functional coatings and high-performance composite material production. The portable design enables it to perform material surface repair or functionalization treatment at industrial sites.

[0040] In summary, the present invention provides a high-precision, low-energy consumption, green and environmentally friendly, and highly adaptable energy-level controllable small laser irradiation grafting and cross-linking system and its application method, which provides a new technical path for surface modification of polymer materials, preparation of high-performance composite materials and manufacturing of precision devices, and has significant application prospects and promotion value. BRIEF DESCRIPTION OF THE DRAWINGS

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

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

[0043] Figure 3 is a schematic diagram of a 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 The energy wave distribution diagram generated by the laser irradiator of the present invention;

[0046] Figure 6 This is a morphology characterization and optical test diagram of the optical lens of the present invention. DETAILED DESCRIPTION

[0047] The present invention relates to a small laser irradiation grafting and cross-linking system with controllable energy levels, aiming to achieve high-precision and high-efficiency modification of the material surface through laser irradiation technology. The specific implementation of the present invention is described in detail below in conjunction with the accompanying drawings and table contents of the specification.

[0048] 1. Embodiment:

[0049] (1) System composition and working principle

[0050] The system of the present 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. Figure 1 As shown, the system realizes full-process automated control of laser irradiation grafting and cross-linking 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, which maintains the laser cavity in the best working state through temperature control to ensure the stability of the laser wavelength and power output.

[0053] The laser beam is introduced into the focusing optical system through optical fiber or free space transmission to ensure the stability and energy consistency of the laser output path. In order to achieve effective integration of the system with external control equipment, power supply system and safety interlock mechanism, the laser irradiator is equipped with a variety of standardized interfaces (such as Figure 4 ), including a remote interlock socket, a USB socket, a general purpose input / output port, and a mains voltage socket.

[0054] like Figure 3 The figure shows a schematic diagram of the laser irradiator of the present invention, which shows the overall structural layout of the laser source and the detailed position distribution of each functional interface. Through this interface design, remote monitoring, data communication, laser start and stop control, and equipment operation status feedback can be realized, improving the convenience of equipment operation and system integration.

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

[0056] Table 1 Technical parameters of laser irradiator

[0057]

[0058] Note: SM stands for single-mode fiber, PM stands for polarization-maintaining fiber, and MM stands for multimode fiber. The system can flexibly configure the fiber output mode according to the processing requirements. Different wavelengths and power configurations can flexibly meet the processing requirements of various materials such as polymers, metals, and ceramics. Digital modulation is up to 150MHz, which is suitable for high-speed modulation processes and enhances pulse laser control capabilities.

[0059] 2. Focusing optical system

[0060] The focusing optical system adopts a high-transmittance quartz lens with an aspherical design (focal length 50mm, numerical aperture NA=0.6) and a high-reflectivity mirror with a gold-plated surface (reflectivity>99.5%). The laser beam is focused on the surface of the material to be processed through the lens, mirror and optical fiber transmission system.

[0061] High-transmittance lens groups and reflectors with anti-reflection coatings, single-lens transmittance >99.8%, and overall optical path efficiency >95% are used to minimize light loss. The dynamic optical path adjustment function is achieved through a piezoelectric ceramic-driven micro-displacement platform, with an X / Y / Z axis displacement accuracy of ±0.1μm, a repeatability accuracy of ±0.05μm, and support for real-time calibration of focus position offset. The optical path calibration algorithm is based on CCD image feedback and automatically corrects the optical path deviation through the Gaussian spot centroid positioning method (positioning error ±0.5μm). The adjustable focus lens has a zoom range of ±10mm, is driven by a stepper motor, and has a step length accuracy of 0.1μm, supporting flexible processing of materials of different thicknesses. The optical path design has been verified by Zemax optical simulation, with a focus spot diameter of <5μm and an energy density distribution uniformity of >90%.

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

[0063] 3. Laser energy control module

[0064] The laser energy control module includes a beam splitter and a power control unit, which supports single pulse, periodic pulse and continuous mode switching. The beam splitter is used to separate the main beam and the reference beam to ensure energy control accuracy. The power control unit can adjust the laser intensity by electrically adjusting the variable iris, polarizer, etc. Figure 5 As shown, the energy waves generated by the laser irradiator can achieve multi-energy level processing through dynamic energy regulation.

[0065] 4. Processing platform

[0066] The processing platform is a three-dimensional mobile platform with a moving accuracy of ±1μm, a maximum travel of 100mm×100mm×50mm, and is equipped with a high-precision positioning system. The platform is connected through a computer or control system to ensure that it moves according to the predetermined path and speed. Figure 2 As shown, the structural schematic diagram of the irradiation system shows how the processing platform and the laser beam work together.

[0067] 5. Chemical reaction auxiliary module

[0068] The chemical reaction auxiliary module integrates a gas environment control system, which realizes the dynamic ratio of nitrogen (N2), oxygen (O2) or argon (Ar) through a high-precision mass flow meter to ensure that the gas composition of the reaction environment is accurately controlled. The system is equipped with a gas purity detection module to monitor the gas purity in real time. When the gas purity is detected to be lower than the set threshold (such as 99.99%), it automatically triggers an alarm and terminates the reaction to ensure the safety and reliability of the experiment. In addition, the system has preset gas modes for different materials, such as:

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

[0070] Metal surface oxidation: Use a mixed gas of oxygen and nitrogen with a flow ratio of O22L / min+N23L / min to optimize the oxidation reaction effect.

[0071] Ceramic activation: Use pure argon environment and set the flow rate to 8L / min to ensure efficient activation of the ceramic surface.

[0072] Through flexible gas ratios and preset modes, the chemical reaction auxiliary module can meet the processing needs of a variety of materials and significantly improve 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 adjustment range is 0.1-10L / min, and the control accuracy is ±0.05L / min; the oxygen flow adjustment range is 0.05-5L / min, and the accuracy is ±0.03L / min. The system can introduce oxygen to promote the occurrence of certain oxidation reactions, and realize the dynamic ratio of N2 / O2 through the gas mixing unit (such as nitrogen accounts for ≥95% in the reduction reaction, and oxygen accounts for 5-50% in the oxidation reaction). For different materials, the system presets gas modes: polypropylene grafting (N2 flow 5L / min), metal surface oxidation (O2 flow 2L / min+N23L / min), and ceramic activation (Ar flow 8L / min). In addition, the system has a built-in gas purity detection module (detection accuracy is ±0.1%). When the gas purity is lower than 99.99%, it will automatically alarm and terminate the reaction.

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

[0075] It includes a K-type thermocouple temperature sensor (measuring range -50~300℃, 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 composed of a CMOS camera (resolution 5MP, positioning error ±1μm). The 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 uses Kalman filtering (multi-sensor data fusion error <1%) and Canny edge detection algorithm (pixel-level error ±0.5px), and the feedback response time is <50ms to achieve dynamic optimization of the processing process.

[0076] 7. Intelligent control system

[0077] The intelligent control system is based on an embedded processor and an integrated software interface, providing parameter setting, data recording and automatic control of the processing process. The system monitors the processing status in real time through temperature sensors, spectral analysis modules and high-definition cameras, and dynamically optimizes laser parameters based on feedback.

[0078] Working principle of this system:

[0079] First, through laser irradiation, an adjustable laser source emits a laser beam suitable for the target material (select the appropriate wavelength, power and pulse width). The laser beam is precisely focused on the surface of the material through the focusing optical system to form a processing area with high energy density. Secondly, under the high-energy irradiation of the laser, the molecules on the surface of the material are excited, and the excited molecules combine with the reactants to form a grafted structure, or form a cross-linked structure through high-energy collision. Then the sample is moved according to the set trajectory through the processing platform to ensure that the laser completes uniform processing in the specified area. The three-dimensional movement function allows multi-level or complex shape grafting and cross-linking treatment. Secondly, it is monitored and adjusted in real time. The temperature of the processing area is detected by the temperature sensor to prevent overheating and material degradation. The spectral analysis module monitors the chemical reaction state in real time to ensure that the grafting and cross-linking are fully completed. The system dynamically adjusts the laser power, pulse width or path according to the feedback data to ensure processing accuracy and stability. Finally, after the processing is completed, the surface morphology and performance data recorded by the monitoring system are used for quality evaluation. Generate a complete data report of the processing process for subsequent process optimization and reference for mass production.

[0080] Through the above composition and working principle, the present invention realizes an efficient, accurate and environmentally friendly material grafting and cross-linking processing process, which is suitable for a variety of application scenarios and material types.

[0081] 2. Specific Application Examples

[0082] (1) Material preparation

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

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

[0085] 3. Photoinitiator: Select ammonium persulfate (APS) with a purity of ≥98%.

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

[0087] 5. Sample pretreatment: Dissolve 10 g of maleic acid in 90 mL of deionized water to prepare a 10 wt.% maleic acid solution. Add ammonium persulfate photoinitiator (concentration is 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 is stable and does not move during laser irradiation. Fixation methods include using mechanical clamps or suction cups.

[0089] 7. Optical detection of materials: Before laser processing, use a spectrometer to detect the light transmittance of the material 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 end of the laser needs to be connected to the focusing optical system (such as lens, reflector, etc.) through an adapter to ensure that the laser beam is accurately transmitted to the material to be processed.

[0092] 2. The laser is transmitted to the focusing lens through optical fiber or free space. Make sure that the optical fiber connection is not loose, and adjust the insertion angle of the optical fiber so that the laser beam is transmitted along the correct path.

[0093] 3. The 3D platform needs to be connected to a computer or control system to ensure that 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 debug its temperature range and control accuracy to ensure that the sample temperature is stable near the set value during processing.

[0094] 4. Install a high-definition camera or infrared camera to monitor the surface status of the sample in real time during laser processing. Use image processing software to obtain the reaction of the sample surface in real time to ensure the uniformity and consistency of processing. Use the CCD camera to collect the focused spot image, use the centroid positioning algorithm to calculate the spot offset, and drive the piezoelectric ceramic platform to compensate for the position deviation within the range of ±0.5μm.

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

[0096] 6. Set the feedback mechanism of parameters such as temperature and power. When the system detects abnormal processing conditions, it automatically adjusts the laser parameters or processing path to ensure that the processing process is always in the best state.

[0097] (3) Experimental operation

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

[0099] 2. Use a micro-spraying system to evenly coat the maleic acid solution on the surface of the PP film, ensuring that the sample surface is completely covered with the MA solution to avoid missing some areas. The coating thickness is controlled within 10μm. After coating, let it stand for 10 minutes to ensure that the solution forms a uniform film on the PP surface.

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

[0101] 4. Under nitrogen protection (flow rate 5 L / min, purity 99.99%), laser scanning was performed on the sample surface with a scanning speed of 5 mm / s and an irradiation time of 3 minutes.

[0102] 5. When the laser beam is irradiated, the three-dimensional platform will move smoothly according to the set path and speed, so that the laser can 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 residues.

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

[0105] (4) Performance evaluation

[0106] 1. Use a scanning electron microscope (SEM) to observe the surface morphology of the PP sample after laser irradiation. Analyze the microstructural changes on the surface of the PP sample to determine whether the grafting reaction is successful.

[0107] 2. Compare the surface morphology before and after treatment to see if any new structure is formed or the surface roughness changes.

[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 to observe whether MA characteristic peaks (such as absorption peaks of functional groups such as 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 by tensile tests, hardness tests, etc. Grafting reactions can usually improve the surface strength, wear resistance and tensile strength of the material.

[0110] 5. The thermal stability of the samples was tested using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The grafting reaction can improve the thermal stability of PP, and the thermal degradation temperature and thermal decomposition characteristics of the samples were analyzed during the test.

[0111] 6. Use solubility test method (such as dissolution in appropriate solvent) or other quantitative methods to determine the grafting degree and verify the effect of PP grafting MA under laser irradiation.

[0112] 3. Experimental Results and Data Analysis

[0113] According to the experimental data, Table 2 shows the comparison of the experimental results of the system of the present invention and the traditional chemical method:

[0114] Table 2 Comparative experimental data table

[0115] index Traditional chemical method The present invention Improvement 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 table in Table 2, the grafting rate of the present invention is 88±3%, which is 35% higher than the 65±5% of the traditional chemical method. The reaction time is shortened from 120 minutes to 8 minutes, and the efficiency is increased by 93%. The energy consumption is reduced from 2.5kWh / kg to 0.3kWh / kg, a reduction of 88%.

[0117] 4. Optimization range of process parameters for different materials

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

[0119] Table 3 Optimization range of process parameters for different materials

[0120]

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

[0122] By integrating the experimental data and process parameter optimization results of Table 2 and Table 3, the energy level controllable small laser irradiation grafting and cross-linking system of the present invention shows significant process advantages in various material application fields. The system adopts a miniaturized design, combined with low energy consumption and high-precision control, and can efficiently handle the surface modification and functional development of high-performance products such as polymer composite materials, electronic devices, and medical materials. Compared with traditional processes, this system has achieved significant improvements in grafting rate, reaction time and energy consumption. For example, the grafting rate has been increased from 65±5% of the traditional chemical method to 88±3%, the reaction time has been shortened from 120 minutes to 8 minutes, and the energy consumption has been reduced from 2.5kWh / kg to 0.3kWh / kg. In addition, the system significantly reduces the energy consumption and pollution risks in the grafting and cross-linking process through green and environmentally friendly processes, providing an innovative solution for achieving green manufacturing of materials.

[0123] The present invention successfully solves multiple technical problems of traditional grafting and cross-linking technologies in terms of reaction control, environmental adaptability, efficiency, material compatibility, processing accuracy and equipment volume through a small laser irradiation grafting and cross-linking system with controllable energy levels. Through precise energy control, modular design and intelligent feedback mechanism, the system significantly improves the efficiency, accuracy and environmental friendliness of material grafting and cross-linking processing. For example, the system supports the processing of a variety of 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 the minimum processing area reaching less than 1μm. This system provides a green, efficient and precise solution for the functionalization of polymer materials and the research and development of high-performance composite materials, and promotes the development of material modification technology in a more intelligent and environmentally friendly direction.

Claims

1. A small laser irradiation grafting and cross-linking system with controllable energy levels, characterized in that: include: An adjustable laser source, which 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, and a built-in temperature control unit; A focusing optical system, which includes a high-transmittance quartz lens with an aspherical design and a high-reflectivity reflector with a gold-plated surface. The laser beam is focused on the surface of the material to be processed through the lens, the reflector and the optical fiber transmission system, and has a dynamic optical path adjustment function; A laser energy control module, which includes a beam splitter and a power control unit, and supports single pulse, periodic pulse and continuous mode switching; The processing platform is a three-dimensional moving platform with high-precision positioning function, a moving accuracy of ±1μm, and a maximum travel of 100mm×100mm×50mm; A chemical reaction auxiliary module, which includes a gas environment control system, realizes dynamic proportioning of nitrogen, oxygen or argon through a mass flow meter, and has gas purity detection and alarm functions; A real-time monitoring and feedback system, comprising a K-type thermocouple temperature sensor, a fiber optic spectrometer and an image analysis module, for real-time monitoring of the temperature, reaction state and surface morphology of the processing area; Intelligent control system, based on embedded processor, integrated software interface, with parameter setting, data recording and process automation control functions.

2. The system according to claim 1, characterized in that The power adjustment accuracy of the adjustable laser source is 0.1 mW.

3. The system according to claim 1, characterized in that The aspherical quartz lens of the focusing optical system has a focal length of 50 mm and a numerical aperture of 0.

6.

4. The system according to claim 1, characterized in that The dynamic optical path adjustment function is realized by a piezoelectric ceramic driven micro-displacement platform, with an X / Y / Z axis displacement accuracy of ±0.1μm and a repeat positioning accuracy of ±0.05μm.

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

6. The system according to claim 1, characterized in that The chemical reaction auxiliary module uses a mass flow meter to achieve a nitrogen flow adjustment range of 0.1L / min to 10L / min and an oxygen flow adjustment range of 0.05L / min to 5L / min.

7. The system according to claim 1, characterized in that The optical fiber spectrometer of the real-time monitoring and feedback system has a wavelength resolution of ±0.1 nm and an integration time of 1 ms to 1000 ms.

8. The system according to claim 1, characterized in that The image analysis module uses a CMOS camera with a resolution of 5MP and a positioning error of ±1μm.

9. The system according to claim 1, characterized in that The intelligent control system has an automatic alarm function, and when it is detected that the gas purity is lower than 99.99% or the processing is abnormal, the system operation is automatically stopped.

10. An application method of the small laser irradiation grafting and cross-linking system with controllable energy levels according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1, material pretreatment, coating the surface of the polypropylene film with maleic acid and photoinitiator solution; 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 nitrogen protection environment, the surface of the material is grafted or cross-linked by laser irradiation; S5. Through real-time monitoring feedback system, dynamically adjust laser parameters to ensure processing accuracy; S6. After irradiation, clean and dry the material, and conduct surface performance testing and evaluation.

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