Method and system for detecting curing degree of thermosetting material

Abstract

The invention discloses a curing degree detection method and system for a thermosetting material, and the method comprises the steps: obtaining a first loss peak frequency of a first thermosetting sample in a completely uncured state, and obtaining a second loss peak frequency of a second thermosetting sample in a completely cured state; determining a curing degree quantitative model according to the first loss peak frequency and the second loss peak frequency; acquiring the current loss peak frequency of the to-be-tested sample; and determining the curing degree of the to-be-tested sample according to the current loss peak frequency and the curing degree quantitative model. Therefore, on one hand, the curing degree detection method is not interfered by external factors, so that the anti-interference capability and the reliability of the detection method are improved, and the stability and the accuracy of a detection result are further improved. On the other hand, only two endpoint samples in a completely uncured state and a completely cured state need to be prepared, so that the detection steps of the detection method are simple, and the detection cost is reduced.

Description

Technical Field

[0001] This application relates to the field of curing degree testing technology, and in particular to a method and system for testing the curing degree of thermosetting materials. Background Technology

[0002] Thermosetting resin-based composites, also known as thermosetting materials, are widely used in various industries due to their excellent mechanical properties and flexible processing capabilities. The degree of cure is one of the key parameters determining the final performance of thermosetting materials; however, current methods for testing the degree of cure suffer from problems such as complex operation and high cost. Summary of the Invention

[0003] To address the aforementioned technical problems, this application provides a method and system for detecting the degree of curing of thermosetting materials.

[0004] According to a first aspect of the present application, a method for detecting the degree of cure of a thermosetting material is provided. The method includes: acquiring a first loss peak frequency of a first thermosetting sample in a completely uncured state, and acquiring a second loss peak frequency of a second thermosetting sample in a completely cured state; determining a degree of cure quantitative model based on the first loss peak frequency and the second loss peak frequency; acquiring the current loss peak frequency of the sample to be tested; and determining the degree of cure of the sample to be tested based on the current loss peak frequency and the degree of cure quantitative model.

[0005] In some embodiments, obtaining the first loss peak frequency of a first thermosetting sample in a completely uncured state includes: performing a dielectric sweep frequency measurement on the first thermosetting sample within a first preset frequency range to obtain a first dielectric spectrum, wherein the first dielectric spectrum is used to characterize the correlation between the dielectric loss factor and frequency of the first thermosetting sample; and determining the first loss peak frequency based on the first dielectric spectrum.

[0006] In some embodiments, the first preset frequency range is from 0.01 Hz to 10 kHz.

[0007] In some embodiments, obtaining the current loss peak frequency of the test sample includes: performing a dielectric sweep frequency measurement on the test sample within a second preset frequency range to obtain a second dielectric spectrum; and determining the current loss peak frequency based on the second dielectric spectrum.

[0008] In some embodiments, the second preset frequency range is from 0.8 × the first loss peak frequency to 1.2 × the second loss peak frequency.

[0009] In some embodiments, the first thermosetting sample, the second thermosetting sample, and the test sample are all standard epoxy resin systems, and the quantitative model for degree of cure is: α1=[(f当前 -f0) / (f1-f0)]×k where α1 characterizes the degree of curing, f 当前 The current loss peak frequency is represented by f0, the first loss peak frequency is represented by f1, the second loss peak frequency is represented by f1, and the correction factor associated with the standard epoxy resin system is represented by k.

[0010] In some embodiments, the first thermosetting sample, the second thermosetting sample, and the test sample are all modified epoxy systems containing toughening agents. The first loss peak frequency, the second loss peak frequency, and / or the current loss peak frequency include the main peak frequency and the secondary peak frequency. The quantitative model for degree of cure is: α2=1-exp(-0.5×K f Wherein, α2 represents the degree of curing, and K f The ratio of the peak frequency of the main peak to the peak frequency of the secondary peak is used to characterize the ratio of the peak frequency of the main peak to the peak frequency of the secondary peak.

[0011] According to a second aspect of the embodiments of this application, a curing degree detection system for thermosetting materials is provided. The curing degree detection system includes: a frequency sweeping device for acquiring a first loss peak frequency of a first thermosetting sample in a completely uncured state, a second loss peak frequency of a second thermosetting sample in a completely cured state, and a current loss peak frequency of a sample to be tested; a determination device for determining a curing degree quantitative model based on the first loss peak frequency and the second loss peak frequency; and a control device including a data processing module and a control module. The data processing module is configured to determine the curing degree of the sample to be tested based on the current loss peak frequency and the curing degree quantitative model, and the control module is configured to control the coordinated operation of the frequency sweeping device, the determination device, and the data processing module.

[0012] In some embodiments, the frequency sweeping device includes an electrode device, the electrode device including two electrode plates disposed opposite each other, and a sample to be tested is placed between the two electrode plates. The sample to be tested includes a first thermosetting sample, a second thermosetting sample, and the sample to be tested. The frequency sweeping device further includes an adjustment mechanism for adjusting the distance between the two electrode plates and the sample to be tested.

[0013] In some embodiments, the control device further includes a verification module, which is used to verify the accuracy of the current loss peak frequency.

[0014] The technical solutions provided by the embodiments of this application may include the following beneficial effects: The curing degree detection method for thermosetting materials provided in this application only requires obtaining the first loss peak frequency of the thermosetting material in a completely uncured state and the second loss peak frequency of the thermosetting material in a completely cured state. Based on the first and second loss peak frequencies, a quantitative model for curing degree is determined. Subsequently, when detecting the curing degree of the test sample, only the current loss peak frequency of the test sample needs to be obtained. Based on the current loss peak frequency and the quantitative model for curing degree, the curing degree of the test sample can be determined.

[0015] Because the loss peak frequency of thermosetting materials continuously shifts from the uncured state to the fully cured state, and there is a clear and quantifiable functional relationship between the shift and the degree of cure of the thermosetting material, and because the frequency shift of the loss peak frequency is an inherent physical property of the material itself and is not affected by external factors, the degree of cure detection method for thermosetting materials in this application establishes a quantitative model of the degree of cure between the loss peak frequency and the degree of cure based on the frequency shift characteristics of the loss peak frequency of thermosetting materials. On the one hand, this makes the degree of cure detection method unaffected by external factors, thereby improving the anti-interference ability and reliability of the detection method, and thus improving the stability and accuracy of the detection results. On the other hand, only two endpoint samples, one in the fully uncured state and one in the fully cured state, are required to simplify the detection steps, enabling rapid detection of the degree of cure of thermosetting materials while also reducing detection costs.

[0016] Other features and advantages of this application will become clear when reading the following description of exemplary embodiments with reference to the accompanying drawings. Attached Figure Description

[0017] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of this application. In these drawings, similar reference numerals are used to denote similar elements. The drawings described below are some embodiments of this application, but not all embodiments. Other drawings will be readily available to those skilled in the art based on these drawings without any inventive effort.

[0018] Figure 1 This is a schematic flowchart illustrating a method for detecting the degree of curing of thermosetting materials according to an exemplary embodiment; Figure 2 This is a schematic flowchart illustrating a method for detecting the degree of curing of thermosetting materials according to another exemplary embodiment; Figure 3 This is a schematic flowchart illustrating a method for detecting the degree of curing of thermosetting materials according to another exemplary embodiment; Figure 4This is a schematic flowchart illustrating a method for detecting the degree of curing of thermosetting materials according to another exemplary embodiment; Figure 5 This is a block diagram illustrating a curing degree detection system for thermosetting materials according to an exemplary embodiment; Figure 6 This is a block diagram of a computer device according to an exemplary embodiment.

[0019] Figure label: 1. Curing degree detection system; 10. Frequency sweeping device; 20. Determination device; 30. Control device; 100. Computer equipment; 101. Computing unit; 102. ROM; 103. RAM; 104. Bus; 105. Input / output interface; 106. Input unit; 107. Output unit; 108. Storage unit; 109. Communication unit. Detailed Implementation

[0020] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application. It should be noted that, unless otherwise specified, the embodiments and features in the embodiments of this application can be arbitrarily combined with each other.

[0021] Thermosetting resin-based composites, also known as thermosetting materials, are widely used in various industries due to their excellent mechanical properties and flexible processing capabilities. The degree of cure is one of the key parameters determining the final performance of thermosetting materials; however, current methods for testing the degree of cure suffer from problems such as complex operation and high cost.

[0022] For example, the curing degree detection method in related technologies involves collecting near-infrared spectra of completely uncured thermosetting material samples and a batch of thermosetting material samples with different degrees of curing, respectively, and measuring their curing degree using the DSC method. Chemometric methods are then used to correlate the near-infrared spectra of the samples with the curing degree index to establish a calibration model. The model's analytical accuracy is improved by selecting different spectral preprocessing methods and choosing different spectral ranges. For detecting the curing degree of unknown samples, simply measuring their near-infrared spectra allows for the measurement of their curing degree based on the established calibration model.

[0023] However, the above-mentioned curing degree detection methods require the acquisition of near-infrared spectra for thermosetting materials with different curing degrees, and the use of complex chemometric methods to establish a calibration model. The operation is complicated and the cost is high.

[0024] To address the aforementioned issues, this application provides a method for detecting the degree of cure of thermosetting materials. This method only requires obtaining the first loss peak frequency of the thermosetting material in a completely uncured state and the second loss peak frequency of the thermosetting material in a completely cured state. Based on the first and second loss peak frequencies, a quantitative model for the degree of cure is determined. Subsequently, when detecting the degree of cure of the test sample, only the current loss peak frequency of the test sample needs to be obtained. Based on the current loss peak frequency and the quantitative model for the degree of cure, the degree of cure of the test sample can be determined.

[0025] Because the loss peak frequency of thermosetting materials continuously shifts from the uncured state to the fully cured state, and there is a clear and quantifiable functional relationship between the shift and the degree of cure of the thermosetting material, and because the frequency shift of the loss peak frequency is an inherent physical property of the material itself and is not affected by external factors, the degree of cure detection method for thermosetting materials in this application establishes a quantitative model of the degree of cure between the loss peak frequency and the degree of cure based on the frequency shift characteristics of the loss peak frequency of thermosetting materials. On the one hand, this makes the degree of cure detection method unaffected by external factors, thereby improving the anti-interference ability and reliability of the detection method, and thus improving the stability and accuracy of the detection results. On the other hand, only two endpoint samples, one in the fully uncured state and one in the fully cured state, are required to simplify the detection steps, enabling rapid detection of the degree of cure of thermosetting materials while also reducing detection costs.

[0026] The method for testing the degree of cure of thermosetting materials provided in this application will be described in detail below with reference to the accompanying drawings.

[0027] This application provides a method for detecting the degree of cure of thermosetting materials, such as... Figure 1 As shown, the method for testing the degree of cure of thermosetting materials includes the following steps: S100: Obtain the first loss peak frequency of the first thermosetting sample in a completely uncured state, and obtain the second loss peak frequency of the second thermosetting sample in a completely cured state.

[0028] In this step, a first thermosetting sample in a completely uncured state and a second thermosetting sample in a completely cured state are first prepared. Then, dielectric frequency sweep measurements are performed on the first and second thermosetting samples to obtain the first loss peak frequency of the first thermosetting sample and the second loss peak frequency of the second thermosetting sample. It is understood that the thermosetting sample refers to a sample of a thermosetting resin-based composite material. The loss peak frequency refers to the voltage frequency corresponding to the peak value of the dielectric loss factor.

[0029] S200. Determine the quantitative model of curing degree based on the first loss peak frequency and the second loss peak frequency.

[0030] In this step, a quantitative model of curing degree is obtained based on the first and second loss peak frequencies to characterize the functional relationship between the loss peak frequency and the curing degree. This model can be obtained through various analysis software, such as dielectric analysis software, modeling software, and general data analysis and curve fitting software. No specific limitations are imposed on this.

[0031] S300: Obtain the current peak loss frequency of the sample to be tested.

[0032] In this step, the current loss peak frequency of the sample under test can also be obtained through dielectric sweep frequency measurement.

[0033] S400. Determine the degree of curing of the sample to be tested based on the current loss peak frequency and curing degree quantitative model.

[0034] In this step, the degree of cure of the test sample is determined based on the current loss peak frequency and the degree of cure quantitative model. The degree of cure quantitative model characterizes the functional relationship between the loss peak frequency and the degree of cure. By inputting the current loss peak frequency into the degree of cure quantitative model, the degree of cure of the test sample can be calculated. The calculation process can be performed manually or automatically using software, data analysis models, etc.

[0035] Because the loss peak frequency of thermosetting materials will continuously shift from the uncured state to the fully cured state, and there is a clear and quantifiable functional relationship between the shift amount and the degree of curing of the thermosetting material, and the frequency shift of the loss peak frequency of thermosetting materials is an inherent physical property of the material itself and is not affected by external factors.

[0036] Based on this, in the curing degree detection method for thermosetting materials in this embodiment, a quantitative curing degree model is established based on the frequency shift characteristics of the loss peak frequency of thermosetting materials. This model ensures that the curing degree detection method is not affected by external factors, thereby improving the anti-interference ability and reliability of the detection method, and ultimately improving the stability and accuracy of the detection results. Furthermore, only two endpoint samples—completely uncured and fully cured—need to be prepared, simplifying the detection steps. This allows for rapid detection of the curing degree of thermosetting materials while also reducing detection costs.

[0037] It should be noted that the first thermosetting sample, the second thermosetting sample, and the test sample in this embodiment are all thermosetting materials, that is, all thermosetting resin-based composite materials. In this embodiment, the resin system of the thermosetting resin-based composite material is not specifically limited. For example, it can be an epoxy resin system, a modified epoxy system, etc., thereby improving the universality of the curing degree detection method.

[0038] In one embodiment, such as Figure 2 As shown, obtaining the first loss peak frequency of the first thermosetting sample in a completely uncured state in step S100 specifically includes the following steps: S110. Dielectric sweep frequency measurement is performed on the first thermosetting sample within a first preset frequency range to obtain the first dielectric spectrum. The first dielectric spectrum is used to characterize the correlation between the dielectric loss factor and frequency of the first thermosetting sample.

[0039] In this step, dielectric sweep frequency measurement can be performed, for example, using a dielectric analyzer. When the dielectric analyzer applies an electric field of a certain frequency to the first thermosetting sample through an electrode device, the dipoles and charges inside the first thermosetting sample will become polarized under the drive of the electric field, and may lose energy due to processes such as friction and scattering, thereby generating a response current with the same frequency as the applied voltage but with a slightly offset phase. This response current is fed back to the dielectric analyzer. Through the above operation, dielectric sweep frequency measurement of the first thermosetting sample is performed within a first preset frequency range. The dielectric analyzer forms a first dielectric spectrum based on the dielectric loss factor of the first thermosetting sample at different frequencies. This first dielectric spectrum is used to characterize the correlation between the dielectric loss factor and frequency of the first thermosetting sample.

[0040] S120. Determine the first loss peak frequency based on the first dielectric spectrum.

[0041] In this step, the first loss peak frequency is determined based on the first dielectric spectrum, that is, the frequency corresponding to the peak value of the dielectric loss factor in the first dielectric spectrum is the first loss peak frequency.

[0042] In this embodiment, the first dielectric spectrum is obtained by performing dielectric sweep frequency measurement on the first thermosetting sample within a first preset frequency range, and then the first loss peak frequency is determined based on the first dielectric spectrum. This simplifies the method of determining the first loss peak frequency, thereby improving the convenience and efficiency of the curing degree detection method.

[0043] In one embodiment, the first preset frequency range is 0.01Hz to 10kHz. Since the loss peak frequency of most thermosetting materials is currently within the range of 0.01Hz to 10kHz, ensuring the width of the first preset frequency range can improve the comprehensiveness of capturing the loss peak frequency of thermosetting materials in different systems. This improves the sensitivity of detecting the loss peak frequency of thermosetting materials, thereby improving the accuracy of the curing degree detection method. On the other hand, it can also further improve the universality of the curing degree detection method.

[0044] In one embodiment, such as Figure 3 As shown, obtaining the current loss peak frequency of the test sample in step S300 specifically includes the following steps: S310. Perform dielectric sweep frequency measurement on the sample to be tested within the second preset frequency range to obtain the second dielectric spectrum.

[0045] In this step, when performing dielectric frequency sweep measurements on the test sample within the second preset frequency range, the measurements can be performed using, for example, the dielectric analyzer described above, and will not be repeated here. For example, the second preset frequency range can be the same as the first preset frequency range, i.e., 0.01Hz to 10kHz, or a different frequency range can be set according to requirements; no specific limitation is made here.

[0046] S320. Determine the current loss peak frequency based on the second dielectric spectrum.

[0047] In this step, the current loss peak frequency is determined based on the second dielectric spectrum, that is, the frequency corresponding to the peak value of the dielectric loss factor in the second dielectric spectrum is the current loss peak frequency.

[0048] In this embodiment, the second dielectric spectrum is obtained by performing dielectric sweep frequency measurement on the test sample within a second preset frequency range, and then the current loss peak frequency is determined based on the second dielectric spectrum. This simplifies the method of determining the current loss peak frequency, thereby improving the convenience and efficiency of the curing degree detection method.

[0049] In one embodiment, the second preset frequency range is from 0.8 × the first loss peak frequency to 1.2 × the second loss peak frequency. Since the first and second loss peak frequencies define the characteristic frequencies of thermosetting materials at two endpoints—the fully uncured state and the fully cured state—when measuring the current loss peak frequency of the test sample, the frequency range of 0.8 × the first loss peak frequency to 1.2 × the second loss peak frequency can dynamically focus on the frequency band where the loss peak frequency is most likely to occur. This allows limited measurement time and resources to be concentrated on the most effective frequency band, reducing noise acquisition in ineffective frequency bands. Consequently, this not only significantly improves the signal-to-noise ratio and reliability of the measurement but also further enhances measurement efficiency.

[0050] In one embodiment, obtaining the second loss peak frequency of the second thermosetting sample in a fully cured state in step S100 specifically includes the following steps: The dielectric frequency sweep measurement of the second thermosetting sample is performed within a third preset frequency range to obtain the third dielectric spectrum, which is used to characterize the correlation between the dielectric loss factor and frequency of the second thermosetting sample.

[0051] Similarly, in this step, dielectric sweep frequency measurement can also be performed, for example, using a dielectric analyzer. Exemplarily, the third preset frequency range is the same frequency range as the first preset frequency range, i.e., 0.01 Hz to 10 kHz.

[0052] The second loss peak frequency is determined based on the third dielectric spectrum.

[0053] In this step, the second loss peak frequency is determined based on the third dielectric spectrum, that is, the frequency corresponding to the peak value of the dielectric loss factor in the third dielectric spectrum is the second loss peak frequency.

[0054] In this embodiment, a third dielectric spectrum is obtained by performing dielectric sweep frequency measurement on the second thermosetting sample within a second preset frequency range, and then the second loss peak frequency is determined based on the third dielectric spectrum. This simplifies the method of determining the second loss peak frequency, thereby improving the convenience and efficiency of the curing degree detection method.

[0055] In one embodiment, when the first thermosetting sample, the second thermosetting sample, and the test sample are all standard epoxy resin systems, the quantitative model for degree of cure is: α1=[(f 当前 -f0) / (f1-f0)]×k Where α1 represents the degree of curing, f 当前 The peak frequency of the current loss is represented by f0, the first peak frequency of the loss is represented by f1, the second peak frequency of the loss is represented by f1, and k represents the correction factor related to the standard epoxy resin system. k is a known parameter in the quantitative model of curing degree, and it can be determined simultaneously in determining the quantitative model of curing degree.

[0056] For example, when f0 is measured to be 50Hz, f1 to be 1200Hz, the second preset frequency range of the test sample is 40Hz to 1500Hz, the current loss peak frequency of the test sample is 600Hz, and k is determined to be 1.02, the degree of curing is calculated as α1 = [(600-50) / (1200-50)] × 1.02 = 0.555. The degree of curing of the test sample is detected by a Differential Scanning Calorimeter (DSC) and found to be 56.1%, with an error of only 0.6% compared to the degree of curing obtained using the degree of curing detection method in this embodiment, which is within an acceptable fluctuation range. This indicates that the degree of curing detection method in this embodiment has high detection accuracy.

[0057] In another embodiment, when the first thermosetting sample, the second thermosetting sample, and the test sample are all modified epoxy systems containing toughening agents, the first loss peak frequency, the second loss peak frequency, and / or the current loss peak frequency include the main peak frequency and the secondary peak frequency, and the degree of cure quantitative model is: α2=1-exp(-0.5×K f ) Where α2 represents the degree of curing, K f It represents the ratio of the peak frequency of the main peak to the peak frequency of the secondary peak.

[0058] For example, the first thermosetting sample exhibits a double peak in its first loss peak frequency, with a main peak frequency of 40 Hz and a secondary peak frequency of 0.5 Hz. The second thermosetting sample has a main peak at 1000 Hz in its second loss peak frequency, and the secondary peak disappears. The measured main peak frequency of the current loss peak frequency of the test sample is 200 Hz, and the secondary peak frequency is 1.0 Hz. K f The value is 200 / 1.0 = 200. At this point, the degree of curing is calculated as α2 = 1 - exp(-0.5 × 200) ≈ 100%. This indicates that the test sample has been completely cured, and the physical phenomenon of the side peaks disappearing is consistent with the model prediction.

[0059] In this embodiment, the corresponding curing degree quantitative model is adjusted for different resin systems, which can further improve the accuracy of curing degree detection for thermosetting materials, thereby improving the reliability of the detection method.

[0060] This application provides a method for detecting the degree of cure of thermosetting materials, such as... Figure 4 As shown, the method for testing the degree of cure of thermosetting materials includes the following steps: S1001. Perform dielectric frequency sweep measurement on the first thermosetting sample within a first preset frequency range to obtain the first dielectric spectrum. The first dielectric spectrum is used to characterize the correlation between the dielectric loss factor and frequency of the first thermosetting sample.

[0061] S1002. Determine the first loss peak frequency based on the first dielectric spectrum.

[0062] S1003. Perform dielectric sweep frequency measurement on the second thermosetting sample within a third preset frequency range to obtain a third dielectric spectrum. The third dielectric spectrum is used to characterize the correlation between the dielectric loss factor and frequency of the second thermosetting sample.

[0063] S1004. Determine the second loss peak frequency based on the third dielectric spectrum.

[0064] S1005. Determine the quantitative model of curing degree based on the first loss peak frequency and the second loss peak frequency.

[0065] S1006. Perform dielectric sweep frequency measurement on the sample to be tested within the second preset frequency range to obtain the second dielectric spectrum.

[0066] S1007. Determine the current loss peak frequency based on the second dielectric spectrum.

[0067] S1008. Determine the degree of curing of the sample to be tested based on the current loss peak frequency and curing degree quantitative model.

[0068] This application provides a curing degree testing system for thermosetting materials, which implements the curing degree testing method described above when applied. Figure 5 As shown, the curing degree detection system 1 includes a frequency sweep device 10, a determination device 20, and a control device 30.

[0069] The frequency sweep device 10 is used to acquire the first loss peak frequency of the first thermosetting sample in a completely uncured state, the second loss peak frequency of the second thermosetting sample in a completely cured state, and the current loss peak frequency of the sample to be tested.

[0070] The determining device 20 is used to determine a quantitative model of the degree of cure based on the first loss peak frequency and the second loss peak frequency. The determining device 20 may be, for example, a device containing dielectric analysis software, modeling software, general data analysis and curve fitting software, etc., and is not specifically limited thereto.

[0071] The control device 30 includes a data processing module and a control module. The data processing module is configured to determine the degree of curing of the test sample based on the current loss peak frequency and a curing degree quantitative model.

[0072] The control module is configured to control the coordinated operation of the frequency sweeping device 10, the determining device 20, and the data processing module. Specifically, the control module first controls the frequency sweeping device 10 to acquire the first loss peak frequency of the first thermosetting sample in a completely uncured state and the second loss peak frequency of the second thermosetting sample in a completely cured state. Then, it controls the determining device 20 to determine the degree of cure quantitative model based on the first and second loss peak frequencies. Subsequently, after controlling the frequency sweeping device 10 to acquire the current loss peak frequency of the sample to be tested, the control module calculates and outputs the degree of cure of the sample to be tested based on the current loss peak frequency and the degree of cure quantitative model.

[0073] The curing degree monitoring system in this embodiment controls the coordinated operation of the frequency sweeping device 10, the determining device 20, and the data processing module through the control module to realize the automatic detection of the curing degree of the test sample, replacing the manual detection method. This greatly improves the efficiency and convenience of curing degree detection and avoids errors caused by uncontrollable factors in manual detection, thereby further improving the accuracy of curing degree detection.

[0074] It should be noted that if the subsequent test samples are from the same resin system as the first test sample, the curing degree quantitative model can be shared. That is, for test samples from the same resin system, starting from the second test sample, the curing degree can be calculated simply by measuring the current loss peak frequency of the test sample.

[0075] In one embodiment, the frequency sweeping device 10 includes a dielectric analyzer and an electrode device, through which a voltage signal within a preset frequency range output by the dielectric analyzer is applied to the sample to be tested. The sample to be tested includes a first thermosetting sample, a second thermosetting sample, and a test sample.

[0076] The electrode device includes two electrode plates arranged opposite each other, with the sample to be tested placed between the two electrode plates. There is a preset gap between the two electrode plates and the sample to be tested. This enables the sweep frequency device 10 in this embodiment to achieve non-contact electrodes, replacing the method of direct contact with the sample to be tested. This avoids problems such as pressure damage to the sample to be tested and short circuits caused by direct contact, thereby further improving the reliability of the curing degree detection system 1.

[0077] To improve the flexibility of the sweep frequency device 10 and thus enhance the versatility of the curing degree detection system 1, the sweep frequency device 10 also includes an adjustment mechanism for adjusting the distance between the two electrode plates and the sample to be tested. This allows the electrode device to be used with samples of different thicknesses and surface conditions.

[0078] For example, the distance between the two electrode plates and the sample to be tested can be adjusted automatically by the control module based on various parameters of the sample to be tested.

[0079] For example, the adjustment mechanism includes two lead screw guides, each including a motor and a lead screw driven by the motor. The lead screw guides also include a guide rod and a nut slidably connected to the guide rod, with the nut also drively connected to the lead screw. Two electrode plates are respectively connected to the two nuts, thus adjusting the distance between the two electrode plates by controlling the electrodes. The adjustment mechanism can also employ other structural forms, such as gear transmission assemblies, without specific limitations, as long as it can adjust the distance between the two electrode plates.

[0080] In one embodiment, the control device 30 further includes a verification module for verifying the accuracy of the current loss peak frequency. The control module pre-stores the variation trajectory of the loss peak frequency for different resin systems. After obtaining the current loss peak frequency of the sample to be tested, it can continuously obtain the current loss peak frequency multiple times. When the current loss peak frequency obtained multiple times exceeds the pre-stored variation trajectory, it is determined that the current loss peak frequency is inaccurate. Since the measurement frequency of the current loss peak frequency is determined based on the first and second loss peak frequencies, when the current loss peak frequency is inaccurate, the control module controls the coordinated operation of the frequency sweeping device 10, the determining device 20, and the data processing module to re-obtain the first and second loss peak frequencies.

[0081] The accuracy of the current loss peak frequency is verified by the verification module, and the first and second loss peak frequencies are reacquired when the current loss peak frequency is inaccurate. This can further improve the accuracy of curing degree detection, thereby further enhancing the reliability of the curing degree detection system 1.

[0082] It should be noted that each module of the aforementioned curing degree detection system can be implemented entirely or partially through software, hardware, or a combination thereof. These modules can be embedded in the processor of a computer device in hardware form or independent of it, or stored in the memory of a computer device in software form, so that the processor can call and execute the corresponding operations of each module.

[0083] In one exemplary embodiment, a computer device is provided, including a processor and a memory, the memory storing a computer program, and the processor executing the computer program to implement the steps of any of the curing degree detection methods described above.

[0084] In one exemplary embodiment, a computer-readable storage medium is provided, on which a computer program is stored, which, when executed by a processor, implements the steps of any of the above-described methods for detecting the degree of hardening. The computer-readable storage medium may be a ROM, random access memory (RAM), CD-ROM, magnetic tape, floppy disk, or optical data storage device, etc.

[0085] In one exemplary embodiment, a computer program product is provided, including a computer program that, when executed by a processor, implements the steps of any of the curing degree detection methods described above.

[0086] refer to Figure 6 The following is a structural block diagram of a computer device that can serve as the curing degree testing system of this application. The computer device 100 includes a computing unit 101, which can perform various appropriate actions and processes according to a computer program stored in a read-only memory (ROM) 102 or a computer program loaded from a storage unit 108 into a random access memory (RAM) 103. The RAM 103 may also store various programs and data required for the operation of the computer device 100. The computing unit 101, ROM 102, and RAM 103 are interconnected via a bus 104. An input / output (I / O) interface 105 is also connected to the bus 104.

[0087] Multiple components in computer device 100 are connected to I / O interface 105, including: input unit 106, output unit 107, storage unit 108, and communication unit 109. Input unit 106 can be any type of device capable of inputting information into computer device 100. Input unit 106 can receive input numerical or character information and generate key signal inputs related to user settings and / or function control of computer device 100, and may include, but is not limited to, a mouse, keyboard, touchscreen, trackpad, trackball, joystick, microphone, and / or remote control. Output unit 107 can be any type of device capable of presenting information, and may include, but is not limited to, a monitor, speaker, video / audio output terminal, vibrator, and / or printer. Storage unit 108 may include, but is not limited to, a hard disk and an optical disk. Communication unit 109 allows computer device 100 to exchange information / data with other devices through computer networks such as the Internet and / or various telecommunications networks, and may include, but is not limited to, modems, network cards, infrared communication devices, wireless communication transceivers, and / or chipsets, such as Bluetooth™ devices, WiFi devices, WiMax devices, cellular communication devices, and / or the like.

[0088] The computing unit 101 can be a variety of general-purpose and / or special-purpose processing components with processing and computing capabilities. Some examples of the computing unit 101 include, but are not limited to, a central processing unit (CPU), a graphics processing unit (GPU), various special-purpose artificial intelligence (AI) computing chips, various computing units running machine learning model algorithms, a digital signal processor (DSP), and any suitable processor, controller, microcontroller, etc. The computing unit 101 performs the various methods and processes described above, such as the firmware detection method. For example, in some embodiments, the firmware detection method may be implemented as a computer software program tangibly contained in a machine-readable medium, such as storage unit 108. In some embodiments, part or all of the computer program may be loaded and / or installed on the computer device 100 via ROM 102 and / or communication unit 109. When the computer program is loaded into RAM 103 and executed by the computing unit 101, one or more steps of the firmware detection method described above may be performed. Alternatively, in other embodiments, the computing unit 101 may be configured to perform the firmware detection method by any other suitable means (e.g., by means of firmware).

[0089] The computer device 100 may be implemented by one or more application-specific integrated circuits (ASICs), digital signal processors (DSPs), digital signal processing devices (DSPDs), programmable logic devices (PLDs), field-programmable gate arrays (FPGAs), controllers, microcontrollers, microprocessors, or other electronic components to perform the curing degree detection method described above.

[0090] The above-described contents can be implemented individually or in various combinations, and these variations are all within the scope of protection of this application.

[0091] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0092] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this application.

Claims

1. A method for detecting the degree of cure of a thermosetting material, characterized in that, The method for detecting the degree of cure of the thermosetting material includes: Obtain the first loss peak frequency of the first thermosetting sample in a completely uncured state, and obtain the second loss peak frequency of the second thermosetting sample in a completely cured state. Based on the first loss peak frequency and the second loss peak frequency, determine the quantitative model of curing degree; Obtain the current loss peak frequency of the test sample; The degree of curing of the test sample is determined based on the current loss peak frequency and the curing degree quantitative model.

2. The method for detecting the degree of cure of thermosetting materials according to claim 1, characterized in that, The process of obtaining the first loss peak frequency of the first thermosetting sample in a completely uncured state includes: The first thermosetting sample is subjected to dielectric sweep frequency measurement within a first preset frequency range to obtain a first dielectric spectrum, which is used to characterize the correlation between the dielectric loss factor and frequency of the first thermosetting sample. The first loss peak frequency is determined based on the first dielectric spectrum.

3. The method for detecting the degree of cure of thermosetting materials according to claim 2, characterized in that, The first preset frequency range is from 0.01 Hz to 10 kHz.

4. The method for detecting the degree of cure of thermosetting materials according to claim 1, characterized in that, The process of obtaining the current loss peak frequency of the test sample includes: The dielectric frequency sweep measurement of the test sample is performed within a second preset frequency range to obtain the second dielectric spectrum; The current loss peak frequency is determined based on the second dielectric spectrum.

5. The method for detecting the degree of cure of thermosetting materials according to claim 4, characterized in that, The second preset frequency range is from 0.8 × the first loss peak frequency to 1.2 × the second loss peak frequency.

6. The method for detecting the degree of cure of thermosetting materials according to claim 1, characterized in that, The first thermosetting sample, the second thermosetting sample, and the test sample are all standard epoxy resin systems, and the quantitative model for degree of cure is: α1=[(f 当前 -f0) / (f1-f0)]×k Wherein, α1 represents the degree of curing, f 当前 The current loss peak frequency is represented by f0, the first loss peak frequency is represented by f1, the second loss peak frequency is represented by f1, and the correction factor associated with the standard epoxy resin system is represented by k.

7. The method for detecting the degree of cure of thermosetting materials according to claim 1, characterized in that, The first thermosetting sample, the second thermosetting sample, and the test sample are all modified epoxy systems containing toughening agents. The first loss peak frequency, the second loss peak frequency, and / or the current loss peak frequency include the main peak frequency and the secondary peak frequency. The quantitative model for degree of cure is: α2=1-exp(-0.5×K f ) Wherein, α2 represents the degree of curing, K f The ratio of the peak frequency of the main peak to the peak frequency of the secondary peak is used to characterize the ratio of the peak frequency of the main peak to the peak frequency of the secondary peak.

8. A system for detecting the degree of cure of thermosetting materials, characterized in that, The curing degree detection system includes: A frequency sweeping device is used to acquire the first loss peak frequency of a first thermosetting sample in a completely uncured state, the second loss peak frequency of a second thermosetting sample in a completely cured state, and the current loss peak frequency of the sample to be tested. The determining device is used to determine a quantitative model of curing degree based on the first loss peak frequency and the second loss peak frequency; A control device, comprising a data processing module and a control module, wherein the data processing module is configured to determine the degree of curing of the test sample based on the current loss peak frequency and the degree of curing quantitative model, and the control module is configured to control the coordinated operation of the frequency sweeping device, the determining device and the data processing module.

9. The curing degree detection system for thermosetting materials according to claim 8, characterized in that, The frequency sweeping device includes an electrode assembly, which includes two opposing electrode plates. A sample to be tested is placed between the two electrode plates. The sample to be tested includes a first thermosetting sample, a second thermosetting sample, and the sample to be tested. The frequency sweeping device further includes: An adjustment mechanism is provided for adjusting the distance between the two electrode plates and the sample to be tested.

10. The curing degree detection system for thermosetting materials according to claim 8, characterized in that, The control device further includes: A verification module is used to verify the accuracy of the current loss peak frequency.

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