In-situ detection method, system, medium and equipment for curing degree of epoxy sample

Abstract

The embodiment of the invention discloses an in-situ detection method, system, medium and equipment for the curing degree of an epoxy sample. The method comprises the following steps: acquiring the internal temperature and environment temperature of the epoxy sample at a preset experimental temperature and experimental time through thermocouples positioned inside and outside the epoxy sample respectively; determining an epoxy sample curing degree initial calculation model according to the internal temperature of the epoxy sample and the environment temperature; determining a convection cooling rate fitting function according to the epoxy sample curing degree initial calculation model; correcting the epoxy sample curing degree initial calculation model through a convection cooling rate fitting function to determine an epoxy sample curing degree optimal calculation model; and obtaining the curing degree of the epoxy sample according to the optimal calculation model of the curing degree of the epoxy sample. An initial calculation model of the curing degree of the epoxy sample is determined through the internal temperature of the epoxy sample and the environment temperature, and the model is corrected through a convection cooling rate fitting function to determine an optimal calculation model of the curing degree of the epoxy sample, so that the curing degree of the epoxy sample is accurately obtained.

Description

Technical Field

[0001] The invention relates to the technical field of curing degree detection of thermosetting epoxy samples, and in particular to an in-situ detection method, system, medium and equipment for the curing degree of epoxy samples. Background Art

[0002] Epoxy materials have excellent bonding properties, corrosion resistance, mechanical properties and electrical insulation properties, and are widely used in electronic device packaging, power equipment insulation, aerospace, construction and transportation. However, poor epoxy resin curing process will produce stress, bubbles, cracks, poor adhesion, delamination and warping, which will reduce the strength and life of the prepared epoxy specimens, or even cause failure. With the development of society and the improvement of economic level, the requirements for the mechanical properties and insulation properties of equipment are getting higher and higher. At home and abroad, filling powders and curing processes are usually compounded and modified to improve the mechanical properties and insulation properties of equipment. However, if the curing time is too long or the reaction temperature is too high, the reaction degree of the epoxy specimen will be too high and gel prematurely; these problems will reduce the performance of the equipment.

[0003] The degree of cure reflects the progress of the epoxy sample curing reaction and is closely related to the physical and chemical changes of the material curing reaction. Therefore, detecting the degree of cure of epoxy samples helps to accurately predict and control the curing reaction of the material, thereby optimizing the curing cycle and manufacturing process. However, the degree of cure test currently usually uses a differential scanning calorimeter, which has high experimental costs, complex operations, and strict test conditions. The traditional differential scanning calorimetry method for epoxy sample formulation and process optimization requires a large number of experiments, and the process control is difficult, so an in-situ measurement method is urgently needed. Summary of the invention

[0004] Based on this, it is necessary to propose an in-situ detection method, system, medium and equipment for the curing degree of epoxy samples in response to the above problems.

[0005] An in-situ detection method for the curing degree of an epoxy sample, the method comprising:

[0006] The internal temperature and ambient temperature of the epoxy specimen at the preset experimental temperature and experimental time are obtained through thermocouples located inside and outside the epoxy specimen respectively.

[0007] An initial calculation model for the curing degree of the epoxy sample is determined according to the internal temperature of the epoxy sample and the ambient temperature.

[0008] The convection cooling rate fitting function is determined according to the initial calculation model of the epoxy sample curing degree.

[0009] The initial calculation model of the curing degree of the epoxy sample is corrected by the convection cooling rate fitting function to determine the optimal calculation model of the curing degree of the epoxy sample.

[0010] The curing degree of the epoxy sample is obtained according to the optimal calculation model for the curing degree of the epoxy sample.

[0011] The initial calculation model for determining the curing degree of the epoxy sample according to the internal temperature of the epoxy sample and the ambient temperature specifically includes:

[0012] The initial convection cooling rate is determined based on the internal temperature of the epoxy sample and the ambient temperature before the start of curing and when the exotherm is zero after curing is completed.

[0013] The heat release during the curing process is determined based on the internal temperature of the epoxy coupon and the ambient temperature during the curing process and the initial convection cooling rate.

[0014] The initial calculation model of the curing degree of the epoxy sample is determined according to the heat released during the curing process.

[0015] The step of determining the heat release during the curing process according to the internal temperature of the epoxy sample and the ambient temperature and the initial convection cooling rate during the curing process specifically includes:

[0016] according to Determine the heat released during the curing process, where H(n) is the heat released in the nth step, C p is the heat capacity of the epoxy sample, T int is the internal temperature of the sample, T env is the ambient temperature, K0 is the initial convection cooling rate, and Δt is the time step of temperature acquisition.

[0017] The initial calculation model for determining the curing degree of the epoxy sample according to the internal temperature of the epoxy sample and the ambient temperature specifically includes:

[0018] according to Determine the initial calculation model of epoxy sample curing degree, where t = n.Δt, t is the current time, n is the number of steps, α RT (t) is the initial calculation model of the curing degree of epoxy sample, H(t) is the heat release at the tth moment, C p is the heat capacity of the epoxy sample, M is the total time, M t is the duration at the tth moment.

[0019] Wherein, determining the convection cooling rate fitting function according to the initial calculation model of the curing degree of the epoxy sample specifically includes:

[0020] The heat flow changes of the epoxy samples at a fixed temperature rise rate were tested by differential scanning calorimetry, and the curing kinetic equation of the epoxy samples was determined according to the heat flow changes.

[0021] Substitute the epoxy sample material temperature into the curing kinetic equation to determine the target calculation model for the epoxy sample curing degree.

[0022] The convection cooling rate fitting function is determined according to the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model.

[0023] The step of substituting the internal temperature of the epoxy sample into the curing kinetic equation to determine the target calculation model for the curing degree of the epoxy sample specifically includes:

[0024] according to Determine the target calculation model for the curing degree of epoxy samples. Among them, α DSC (t) is the target calculation model for the curing degree of epoxy samples, α DSC The curing degree of the epoxy sample is calculated by the curing degree target model, ΔE a is the activation energy, T is the temperature of the epoxy sample material during the curing process, A is the frequency factor of the reaction model, R is the universal gas constant, and m and n are the reaction orders of the reaction model.

[0025] Wherein, determining the convection cooling rate fitting function according to the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model specifically includes:

[0026] By K(t) = f(α RT (t)-α DSC (t)) determines the convective cooling rate fitting function; where K(t) is the convective cooling rate fitting function, α RT (t) is the initial calculation model of epoxy sample curing degree, α DSC (t) is the target calculation model for the degree of curing of epoxy samples.

[0027] The method of correcting the initial calculation model of the curing degree of the epoxy sample by the convection cooling rate fitting function to determine the optimal calculation model of the curing degree of the epoxy sample specifically includes:

[0028] The error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree is determined by the convection cooling rate fitting function.

[0029] The initial calculation model of the epoxy sample curing degree is corrected by the convection cooling rate fitting function until the error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree is minimized, thereby obtaining the optimal convection cooling rate fitting function.

[0030] The initial convection cooling rate in the initial calculation model of the curing degree of the epoxy sample is replaced by the optimal convection cooling rate fitting function to determine the optimal calculation model of the curing degree of the epoxy sample.

[0031] An in-situ detection system for epoxy sample curing degree, the system comprising:

[0032] The internal temperature and ambient temperature acquisition module is used to obtain the internal temperature and ambient temperature of the epoxy sample under the preset experimental temperature and experimental time through thermocouples located inside and outside the epoxy sample respectively.

[0033] The module for determining the initial calculation model of the curing degree of the epoxy sample is used to determine the initial calculation model of the curing degree of the epoxy sample according to the internal temperature of the epoxy sample and the ambient temperature.

[0034] The convection cooling rate fitting function determination module is used to determine the convection cooling rate fitting function according to the initial calculation model of the epoxy sample curing degree.

[0035] The module for determining the optimal calculation model of the curing degree of epoxy samples is used to correct the initial calculation model of the curing degree of epoxy samples by using the convection cooling rate fitting function to determine the optimal calculation model of the curing degree of epoxy samples.

[0036] The epoxy sample curing degree acquisition module is used to obtain the epoxy sample curing degree through the epoxy sample curing degree optimal calculation model.

[0037] A computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the processor executes the steps of the method described above.

[0038] A computer device comprises a memory and a processor, wherein the memory stores a computer program, and when the computer program is executed by the processor, the processor executes the steps of the above method.

[0039] The embodiments of the present invention have the following beneficial effects:

[0040] The present invention directly measures the internal temperature of the epoxy sample during the curing process through an internal thermocouple, obtains the ambient temperature through an external thermocouple, and preliminarily establishes an initial calculation model for the curing degree of the epoxy sample based on the measured internal temperature of the epoxy sample and the ambient temperature. Furthermore, the convection cooling rate fitting function is introduced into the initial calculation model for the curing degree of the epoxy sample, and the initial calculation model for the curing degree of the epoxy sample is corrected, which can eliminate or reduce the error caused by the heat exchange process, determine the optimal calculation model for the curing degree of the epoxy sample, and thus obtain the curing degree of the epoxy sample in real time and accurately based on the optimal calculation model for the curing degree of the epoxy sample. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0042] in:

[0043] Figure 1 A schematic flow chart of an embodiment of an in-situ detection method for the curing degree of an epoxy sample provided by the present invention;

[0044] Figure 2 It is a structural schematic diagram of an embodiment of a thermocouple experimental platform;

[0045] Figure 3 A schematic flow chart of another embodiment of an in-situ detection method for the curing degree of an epoxy sample provided by the present invention;

[0046] Figure 4 A schematic structural diagram of an embodiment of an in-situ detection system for epoxy sample curing degree provided by the present invention;

[0047] Figure 5 A schematic diagram of the structure of an embodiment of the device provided by the present invention;

[0048] Figure 6 A schematic structural diagram of an embodiment of the medium provided by the present invention. DETAILED DESCRIPTION

[0049] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0050] like Figure 1 As shown, Figure 1 A schematic flow chart of an embodiment of an in-situ detection method for the curing degree of an epoxy sample provided by the present invention. An in-situ detection method for the curing degree of an epoxy sample, the method comprising:

[0051] S101: Obtaining the internal temperature and ambient temperature of the epoxy sample at a preset experimental temperature and experimental time through thermocouples located inside and outside the epoxy sample respectively.

[0052] Exemplarily, an epoxy sample is first prepared, and the epoxy sample formula includes: bisphenol A type E-51 epoxy resin (epoxy equivalent is 169-181g / eq), curing agent methyl tetrahydrophthalic anhydride, α-type electrical Al2O3, and accelerator 2,4,6 tris (dimethylaminomethyl) phenol. Among them, the mass ratio of epoxy resin, curing agent, Al2O3 filler and accelerator is 1:1:3:0.02. The above materials are mixed and stirred evenly, and cured at 130°C for 28 hours to prepare the sample.

[0053] Furthermore, the internal temperature and ambient temperature of the epoxy sample are obtained according to the thermocouple experimental platform. Figure 2 , Figure 2 The schematic diagram of the structure of an embodiment of a thermocouple experimental platform. The thermocouple experimental platform includes a temperature recorder, two thermocouples, a constant temperature box, a computer, and a USB data transmission line. Specifically, the two thermocouples are located inside and around the epoxy sample, respectively. The temperature of the thermocouples is transmitted to the computer through the temperature recorder via the USB data transmission line. The temperature recorder can simultaneously collect the temperature of the two thermocouples in real time. The constant temperature box is used to set the preset experimental temperature and experimental time of the curing process. The internal temperature and ambient temperature of the epoxy sample under the preset experimental temperature and experimental time are obtained through the two thermocouples located inside and outside the epoxy sample, respectively.

[0054] It should be noted that the in-situ detection method for the curing degree of an epoxy sample provided by the present invention is not limited to the above-mentioned epoxy sample formula and curing process.

[0055] S102: Determine an initial calculation model for the curing degree of the epoxy sample according to the internal temperature of the epoxy sample and the ambient temperature.

[0056] Exemplarily, the initial convection cooling rate is determined based on the internal temperature of the epoxy sample and the ambient temperature before the start of curing and when the heat release is zero after the curing is completed; the heat release during the curing process is determined based on the internal temperature of the epoxy sample and the ambient temperature and the initial convection cooling rate; and the initial calculation model for the curing degree of the epoxy sample is determined based on the heat release during the curing process.

[0057] Specifically, the initial calculation model of the curing degree of the epoxy sample is determined according to the formula shown below;

[0058]

[0059] Where t = n·Δt, n is the number of steps, α RT (t) is the initial calculation model of the curing degree of epoxy sample, H(t) is the heat release at the tth moment, C p is the heat capacity of the epoxy sample, M is the total time, M t is the duration at the tth moment.

[0060] S103: Determine a convection cooling rate fitting function according to an initial calculation model of the epoxy sample curing degree.

[0061] Exemplarily, the heat flow changes of the epoxy sample at three heating rates (such as 3K / min, 7K / min and 11K / min) are tested by differential scanning calorimetry, and the curing kinetic equation of the epoxy sample, that is, the relationship between the curing degree and time and temperature, is determined according to the heat flow change; the internal temperature of the epoxy sample is substituted into the curing kinetic equation to determine the target calculation model of the curing degree of the epoxy sample. The target calculation model of the curing degree of the epoxy sample is shown as follows:

[0062]

[0063] Among them, α DSC (t) is the target calculation model for the curing degree of epoxy samples, α DSC The curing degree of the epoxy sample is calculated by the curing degree target model, ΔE a is the activation energy, T is the temperature of the epoxy sample material during the curing process, A is the frequency factor of the reaction model, R is the universal gas constant, and m and n are the reaction orders of the reaction model.

[0064] Furthermore, the convection cooling rate fitting function is determined according to the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree. The convection cooling rate fitting function is shown in the following formula:

[0065] K(t)=f(α RT (t)-α DSC (t))(3);

[0066] Where K(t) is the convective cooling rate fitting function, α RT (t) is the initial calculation model of epoxy sample curing degree, α DSC (t) is the target calculation model for the degree of curing of epoxy samples.

[0067] S104: Correcting the initial calculation model of the curing degree of the epoxy sample by using the convection cooling rate fitting function to determine the optimal calculation model of the curing degree of the epoxy sample.

[0068] Exemplarily, the error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree is determined by the convection cooling rate fitting function; the initial calculation model of the epoxy sample curing degree is corrected by the convection cooling rate fitting function until the error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree is minimized, thereby obtaining the optimal convection cooling rate fitting function; the initial convection cooling rate in the initial calculation model of the epoxy sample curing degree is replaced by the optimal convection cooling rate fitting function, thereby determining the optimal calculation model of the epoxy sample curing degree.

[0069] S105: Obtaining the curing degree of the epoxy sample according to the optimal calculation model of the curing degree of the epoxy sample.

[0070] Exemplarily, the corrected optimal calculation model for the curing degree of epoxy samples is used to perform in-situ detection of the curing degree of epoxy samples, thereby improving the test accuracy of in-situ detection of the curing degree by thermocouples.

[0071] From the above description, it can be known that the present invention directly measures the internal temperature of the epoxy sample during the curing process through an internal thermocouple, obtains the ambient temperature through an external thermocouple, and preliminarily establishes an initial calculation model for the curing degree of the epoxy sample based on the measured internal temperature of the epoxy sample and the ambient temperature. Furthermore, the convection cooling rate fitting function is introduced into the initial calculation model for the curing degree of the epoxy sample, and the initial calculation model for the curing degree of the epoxy sample is corrected, which can eliminate or reduce the error caused by the heat exchange process, determine the optimal calculation model for the curing degree of the epoxy sample, and thus obtain the curing degree of the epoxy sample in real time and accurately based on the optimal calculation model for the curing degree of the epoxy sample.

[0072] like Figure 3 As shown, Figure 3 A schematic flow chart of another embodiment of an in-situ detection method for the curing degree of an epoxy sample provided by the present invention. An in-situ detection method for the curing degree of an epoxy sample, the method comprising:

[0073] S201: Obtaining the internal temperature and ambient temperature of the epoxy sample at a preset experimental temperature and experimental time through thermocouples located inside and outside the epoxy sample respectively.

[0074] It should be noted that step S201 Figure 1 This has been discussed in detail in the implementation scenario shown and will not be repeated here.

[0075] S202: Determine the initial convection cooling rate according to the internal temperature of the epoxy sample and the ambient temperature before the start of curing and when the heat release is zero after the curing is completed.

[0076] For example, assuming that the heat dissipated to the surrounding environment is proportional to the temperature difference between the epoxy sample and the environment, the change in the internal temperature of the epoxy sample according to the law of thermal equilibrium is as follows:

[0077] dT int / dt=H(t) / C p -K c ·(T int (t)-T env (t)) (4);

[0078] Among them, T int is the internal temperature of the sample, T env is the ambient temperature, t is the current moment, C pis the heat capacity of the epoxy sample (assuming it is a constant in each test), K C is the convection cooling rate. When the epoxy insulation material no longer generates heat, that is, the heat released before the start of curing and after the completion of curing is zero (H(t) = 0), then equation (4) becomes:

[0079] dT int / dt=-K0·(T int (t)-(T int (t)) (5);

[0080] Where K0 is the initial convective cooling rate, T int is the internal temperature of the sample, T env is the ambient temperature, and t is the current time.

[0081] S203: Determine the heat released during the curing process based on the internal temperature of the epoxy sample and the ambient temperature during the curing process and the initial convection cooling rate.

[0082] Exemplarily, the heat released during the curing process is determined according to the following formula:

[0083] H(t) / C p =T int (t)-T int (t-1)+K0·(T int (t)-T env (t)) (6);

[0084] Where H(t) is the heat released at time t, C p is the heat capacity of the epoxy sample, T int is the internal temperature of the sample, T env is the ambient temperature, K0 is the initial convection cooling rate.

[0085] Considering the data sampling rate of the temperature recorder, if the time step is too long, the temperature is not constant within the given time step; if the time step is too short, the temperature does not change. Therefore, it is necessary to set the time step Δt and use the average temperature at the start and end of the given time step to calculate H(n) / C p , formula (6) is reorganized into formula (7), as shown below:

[0086]

[0087] Where H(n) is the heat released in the nth step, C p is the heat capacity of the epoxy sample, T int is the internal temperature of the sample, T env is the ambient temperature, K0 is the initial convection cooling rate, and Δt is the time step of temperature acquisition.

[0088] S204: Determine an initial calculation model for the curing degree of the epoxy sample according to the heat released during the curing process.

[0089] Exemplarily, the initial calculation model of the curing degree of the epoxy sample is determined according to the formula shown below;

[0090]

[0091] Where t = n·Δt, n is the number of steps, α RT (t) is the initial calculation model of the curing degree of epoxy sample, H(t) is the heat release at the tth moment, C p is the heat capacity of the epoxy sample, M is the total time, M t is the duration at the tth moment, ΔH(t) is the cumulative heat release at the tth moment, H total is the total heat release at time t.

[0092] S205: Testing the heat flow change of the epoxy samples at a fixed temperature rise rate by differential scanning calorimetry, and determining the curing kinetic equation of the epoxy samples according to the heat flow change.

[0093] Exemplarily, the heat flow changes of epoxy samples at three heating rates (such as 3K / min, 7K / min and 11K / min) are tested by differential scanning calorimetry, and the curing kinetic equation of the epoxy sample, that is, the relationship between the degree of curing and time and temperature, is determined based on the heat flow change.

[0094] S206: Substitute the epoxy sample material temperature into the curing kinetic equation to determine the target calculation model for the epoxy sample curing degree.

[0095] Exemplarily, the temperature of the epoxy sample material during the curing process is substituted into the curing kinetic equation to determine the target calculation model for the curing degree of the epoxy sample. The target calculation model for the curing degree of the epoxy sample is shown in the following formula:

[0096]

[0097] Among them, α DSC (t) is the target calculation model for the curing degree of epoxy samples, α DSC The curing degree of the epoxy sample is calculated by the curing degree target model, ΔE a is the activation energy, T is the temperature of the epoxy sample material during the curing process, A is the frequency factor of the reaction model, R is the universal gas constant, and m and n are the reaction orders of the reaction model.

[0098] S207: Determine a convection cooling rate fitting function according to an initial calculation model for the epoxy sample curing degree and a target calculation model for the epoxy sample curing degree.

[0099] Exemplarily, the convection cooling rate fitting function is determined according to the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model, and the convection cooling rate fitting function is shown in the following formula:

[0100] K(t)=f(α RT (t)-α DSC (t))(10);

[0101] Where K(t) is the convective cooling rate fitting function, α RT (t) is the initial calculation model of epoxy sample curing degree, α DSC (t) is the target calculation model for the degree of curing of epoxy samples.

[0102] S208: Determine the error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree through a convection cooling rate fitting function.

[0103] S209: Correcting the initial calculation model of the epoxy sample curing degree by using the convection cooling rate fitting function until the error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree is minimized, thereby obtaining the optimal convection cooling rate fitting function.

[0104] S210: replacing the initial convection cooling rate in the initial calculation model of the curing degree of the epoxy sample with the optimal convection cooling rate fitting function, and determining the optimal calculation model of the curing degree of the epoxy sample.

[0105] S211: Obtaining the curing degree of the epoxy sample according to the optimal calculation model of the curing degree of the epoxy sample.

[0106] It should be noted that steps S208-S211 are Figure 1 This has been discussed in detail in the implementation scenario shown and will not be repeated here.

[0107] From the above description, it can be seen that the present invention can realize in-situ measurement of the curing degree of epoxy materials with different formulas and processes through thermocouples located inside and outside the epoxy sample respectively, and has the advantages of low detection cost, simple and convenient operation, high sensitivity, safety and reliability.

[0108] like Figure 4 As shown, Figure 4 The present invention provides a schematic diagram of an embodiment of an in-situ detection system for the curing degree of epoxy samples. An in-situ detection system 10 for the curing degree of epoxy samples includes:

[0109] The internal temperature and ambient temperature acquisition module 11 is used to acquire the internal temperature and ambient temperature of the epoxy sample at a preset test temperature and test time through thermocouples located inside and outside the epoxy sample respectively.

[0110] The epoxy sample curing degree initial calculation model determination module 12 is used to determine the epoxy sample curing degree initial calculation model according to the epoxy sample internal temperature and the ambient temperature.

[0111] The convection cooling rate fitting function determination module 13 is used to determine the convection cooling rate fitting function according to the initial calculation model of the curing degree of the epoxy sample.

[0112] The module 14 for determining the optimal calculation model of the curing degree of epoxy samples is used to calibrate the initial calculation model of the curing degree of epoxy samples by using the convection cooling rate fitting function to determine the optimal calculation model of the curing degree of epoxy samples.

[0113] The epoxy sample curing degree acquisition module 15 is used to obtain the epoxy sample curing degree through the epoxy sample curing degree optimal calculation model.

[0114] Exemplarily, in the internal temperature and ambient temperature acquisition module 11, the internal temperature and ambient temperature of the epoxy sample at the preset experimental temperature and experimental time are acquired by thermocouples located inside and outside the epoxy sample respectively; in the epoxy sample curing degree initial calculation model determination module 12, the initial convection cooling rate is determined according to the internal temperature and ambient temperature of the epoxy sample before the start of curing and when the heat release is zero after the curing is completed; the heat release during the curing process is determined according to the internal temperature and ambient temperature of the epoxy sample and the initial convection cooling rate during the curing process; the initial calculation model of the curing degree of the epoxy sample is determined according to the heat release during the curing process. In the convection cooling rate fitting function determination module 13, the heat flow change of the epoxy sample at a fixed temperature rise rate is tested by differential scanning calorimetry, and the curing kinetic equation of the epoxy sample is determined according to the heat flow change; the epoxy sample material temperature is substituted into the curing kinetic equation to determine the curing degree target calculation model of the epoxy sample; the convection cooling rate fitting function is determined according to the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model. In the epoxy sample curing degree optimal calculation model determination module 14, the error between the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model is determined by the convection cooling rate fitting function; the epoxy sample curing degree initial calculation model is corrected by the convection cooling rate fitting function until the error between the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model is minimized, and the optimal convection cooling rate fitting function is obtained; the initial convection cooling rate in the epoxy sample curing degree initial calculation model is replaced with the optimal convection cooling rate fitting function, and the epoxy sample curing degree optimal calculation model is determined. In the epoxy sample curing degree acquisition module 15, the epoxy sample curing degree is obtained by the epoxy sample curing degree optimal calculation model.

[0115] like Figure 5 As shown, Figure 5The device 20 includes a memory 21 and a processor 22. The memory 21 stores a computer program, and the processor 22 executes the computer program when working to implement the following. Figure 1 and Figure 3 The method shown.

[0116] The specific technical details of the in-situ detection method of the curing degree of an epoxy sample implemented when the above-mentioned device 20 executes the computer program have been discussed in detail in the aforementioned method steps, so they will not be repeated here.

[0117] like Figure 6 As shown, Figure 6 The structure diagram of an embodiment of the medium provided by the present invention is shown in FIG. The medium 30 stores at least one computer program 31, and the computer program 31 is executed by the processor 22 to implement the following Figure 1 and Figure 3 In one embodiment, the medium 30 may be a storage chip, a hard disk, a mobile hard disk, a USB flash drive, an optical disk, or other readable and writable storage tools, or a server, etc.

[0118] The above describes specific embodiments of the present specification, and other embodiments are within the scope of the appended claims. In some cases, the actions or steps recorded in the claims can be performed in an order different from that in the embodiments and still achieve the desired results. In addition, the processes depicted in the accompanying drawings do not necessarily have to be performed in the specific order or sequential order shown to achieve the desired results. In some embodiments, multitasking and parallel processing are also possible or may be advantageous.

[0119] Each embodiment in this specification is described in a progressive manner, and the same or similar parts between the embodiments can be referred to each other, and each embodiment focuses on the differences from other embodiments. In particular, for the device, equipment, and non-volatile computer-readable storage medium embodiments, since they are basically similar to the method embodiments, the description is relatively simple, and the relevant parts can be referred to the partial description of the method embodiments.

[0120] The apparatus, device, non-volatile computer-readable storage medium and method provided in the embodiments of this specification correspond to each other, and therefore, the apparatus, device, and non-volatile computer storage medium also have similar beneficial technical effects as the corresponding methods. Since the beneficial technical effects of the methods have been described in detail above, the beneficial technical effects of the corresponding apparatus, device, and non-volatile computer storage medium will not be repeated here.

[0121] The systems, devices, modules or units described in the above embodiments may be implemented by computer chips or entities, or by products with certain functions. A typical implementation device is a computer. Specifically, the computer may be, for example, a personal computer, a laptop computer, a cellular phone, a camera phone, a smart phone, a personal digital assistant, a media player, a navigation device, an email device, a game console, a tablet computer, a wearable device, or a combination of any of these devices.

[0122] For the convenience of description, the above device is described by being divided into various units according to their functions and described separately. Of course, when implementing this specification, the functions of each unit can be implemented in one or more software and / or hardware. It should be understood by those skilled in the art that this specification embodiment can be provided as a method, system, or computer program product. Therefore, this specification embodiment can adopt the form of a complete hardware embodiment, a complete software embodiment, or an embodiment combining software and hardware. Moreover, this specification embodiment can adopt the form of a computer program product implemented on one or more computer-usable storage media (including but not limited to disk storage, CD-ROM, optical storage, etc.) containing computer-usable program code.

[0123] This specification is described with reference to the flowcharts and / or block diagrams of the methods, devices (systems), and computer program products according to the embodiments of this specification. It should be understood that each process and / or box in the flowchart and / or block diagram, as well as the combination of the processes and / or boxes in the flowchart and / or block diagram, can be implemented by computer program instructions. These computer program instructions can be provided to a processor of a general-purpose computer, a special-purpose computer, an embedded processor, or other programmable data processing device to produce a machine, so that the instructions executed by the processor of the computer or other programmable data processing device generate instructions for implementing the processes in the flowchart and / or block diagram. Figure 1 A process or multiple processes and / or boxes Figure 1 A device that provides the functions specified in a block or multiple blocks.

[0124] These computer program instructions may also be stored in a computer-readable memory capable of directing a computer or other programmable data processing device to operate in a specific manner, so that the instructions stored in the computer-readable memory produce an article of manufacture comprising an instruction device, which implements the process Figure 1 A process or multiple processes and / or boxes Figure 1 A function specified in one or more boxes.

[0125] These computer program instructions can also be loaded onto a computer or other programmable data processing device so that a series of operating steps are executed on the computer or other programmable device to produce a computer-implemented process, thereby providing instructions for implementing the process. Figure 1 A process or multiple processes and / or boxes Figure 1 The steps for the functions specified in one or more boxes.

[0126] In a typical configuration, a computing device includes one or more processors (CPU), input / output interfaces, network interfaces, and memory.

[0127] The memory may include non-permanent storage in a computer-readable medium, random access memory (RAM) and / or non-volatile memory in the form of read-only memory (ROM) or flash RAM. The memory is an example of a computer-readable medium.

[0128] Computer readable media include permanent and non-permanent, removable and non-removable media that can be implemented by any method or technology to store information. Information can be computer readable instructions, data structures, program modules or other data. Examples of computer storage media include, but are not limited to, phase change memory (PRAM), static random access memory (SRAM), dynamic random access memory (DRAM), other types of random access memory (RAM), read-only memory (ROM), electrically erasable programmable read-only memory (EEPROM), flash memory or other memory technology, compact disk read-only memory (CD-ROM), digital versatile disk (DVD) or other optical storage, magnetic cassettes, magnetic disk storage or other magnetic storage devices or any other non-transmission media that can be used to store information that can be accessed by a computing device. As defined herein, computer readable media does not include temporary computer readable media (transitory media), such as modulated data signals and carrier waves.

[0129] It should also be noted that the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, commodity or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, commodity or device. In the absence of more restrictions, the elements defined by the sentence "comprises a ..." do not exclude the existence of other identical elements in the process, method, commodity or device including the elements.

[0130] This specification may be described in the general context of computer-executable instructions executed by a computer, such as program modules. Generally, program modules include routines, programs, objects, components, data structures, etc. that perform specific tasks or implement specific abstract data types. This specification may also be practiced in distributed computing environments where tasks are performed by remote processing devices connected through a communication network. In a distributed computing environment, program modules may be located in local and remote computer storage media, including storage devices.

[0131] Each embodiment in this specification is described in a progressive manner, and the same or similar parts between the embodiments can be referred to each other, and each embodiment focuses on the differences from other embodiments. In particular, for the system embodiment, since it is basically similar to the method embodiment, the description is relatively simple, and the relevant parts can be referred to the partial description of the method embodiment.

[0132] The above disclosure is only the preferred embodiment of the present invention, which certainly cannot be used to limit the scope of the present invention. Therefore, equivalent changes made according to the claims of the present invention are still within the scope of the present invention.

Claims

1. An in-situ detection method for the curing degree of an epoxy sample, characterized in that: The method comprises: The internal temperature and ambient temperature of the epoxy sample at the preset test temperature and test time are obtained through thermocouples located inside and outside the epoxy sample respectively; Determine an initial calculation model for the curing degree of the epoxy sample according to the internal temperature of the epoxy sample and the ambient temperature; Determining a convection cooling rate fitting function according to the initial calculation model of the epoxy sample curing degree; Correcting the initial calculation model of the epoxy sample curing degree by using the convection cooling rate fitting function to determine the optimal calculation model of the epoxy sample curing degree; The curing degree of the epoxy sample is obtained according to the optimal calculation model for the curing degree of the epoxy sample.

2. The in-situ detection method of the curing degree of an epoxy sample according to claim 1, characterized in that: The initial calculation model for determining the curing degree of the epoxy sample according to the internal temperature of the epoxy sample and the ambient temperature specifically includes: Determine the initial convection cooling rate based on the internal temperature of the epoxy sample and the ambient temperature before the start of curing and when the heat release is zero after the curing is completed; Determining the heat released during the curing process based on the internal temperature of the epoxy sample and the ambient temperature and the initial convection cooling rate during the curing process; The initial calculation model of the curing degree of the epoxy sample is determined according to the heat released during the curing process.

3. The in-situ detection method of the curing degree of an epoxy sample according to claim 2, characterized in that: Determining the heat release during the curing process according to the internal temperature of the epoxy sample and the ambient temperature and the initial convection cooling rate during the curing process specifically includes: according to Determine the heat released during the curing process, where H(n) is the heat released in the nth step, C p is the heat capacity of the epoxy sample, T int is the internal temperature of the sample, T env is the ambient temperature, K0 is the initial convection cooling rate, and Δt is the time step of temperature acquisition.

4. The in-situ detection method of the curing degree of an epoxy sample according to claim 3, characterized in that: The initial calculation model for determining the curing degree of the epoxy sample according to the internal temperature of the epoxy sample and the ambient temperature specifically includes: according to Determine the initial calculation model of epoxy sample curing degree, where t = n·Δt, t is the current time, n is the number of steps, α RT (t) is the initial calculation model of the curing degree of epoxy sample, H(t) is the heat release at the tth moment, C p is the heat capacity of the epoxy sample, M is the total time, M t is the duration at the tth moment.

5. The in-situ detection method of the curing degree of an epoxy sample according to claim 4, characterized in that: The step of determining the convection cooling rate fitting function according to the initial calculation model of the epoxy sample curing degree specifically includes: The heat flow changes of the epoxy samples at a fixed temperature rise rate are tested by differential scanning calorimetry, and the curing kinetic equation of the epoxy samples is determined according to the heat flow changes; Substituting the temperature of the epoxy sample material into the curing kinetic equation to determine the target calculation model for the curing degree of the epoxy sample; The convection cooling rate fitting function is determined according to the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model.

6. The in-situ detection method of the curing degree of an epoxy sample according to claim 5, characterized in that: Substituting the internal temperature of the epoxy sample into the curing kinetic equation to determine the target calculation model for the curing degree of the epoxy sample specifically includes: according to Determine the target calculation model for the degree of curing of epoxy samples; Among them, α DSC (t) is the target calculation model for the curing degree of epoxy samples, α DSC The curing degree of the epoxy sample is calculated by the curing degree target model, ΔE a is the activation energy, T is the temperature of the epoxy sample material during the curing process, A is the frequency factor of the reaction model, R is the universal gas constant, and m and n are the reaction orders of the reaction model.

7. The in-situ detection method of the curing degree of an epoxy sample according to claim 6, characterized in that: The step of determining the convection cooling rate fitting function according to the epoxy sample curing degree initial calculation model and the epoxy sample curing degree target calculation model specifically includes: By K(t)=f(α RT (t)-α DSC (t)) determine the convective cooling rate fitting function; Where K(t) is the convective cooling rate fitting function, α RT (t) is the initial calculation model of epoxy sample curing degree, α DSC (t) is the target calculation model for the degree of curing of epoxy samples.

8. The in-situ detection method of the curing degree of an epoxy sample according to claim 7, characterized in that: The method of correcting the initial calculation model of the curing degree of the epoxy sample by the convection cooling rate fitting function to determine the optimal calculation model of the curing degree of the epoxy sample specifically includes: Determining the error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree by using the convection cooling rate fitting function; Correcting the initial calculation model of the epoxy sample curing degree by using the convection cooling rate fitting function until the error between the initial calculation model of the epoxy sample curing degree and the target calculation model of the epoxy sample curing degree is minimized, thereby obtaining an optimal convection cooling rate fitting function; The initial convection cooling rate in the initial calculation model of the curing degree of the epoxy sample is replaced by the optimal convection cooling rate fitting function to determine the optimal calculation model of the curing degree of the epoxy sample.

9. An in-situ detection system for epoxy sample curing degree, characterized in that: The system comprises: An internal temperature and ambient temperature acquisition module is used to acquire the internal temperature and ambient temperature of the epoxy sample at a preset test temperature and test time through thermocouples located inside and outside the epoxy sample respectively; An epoxy sample curing degree initial calculation model determination module is used to determine the epoxy sample curing degree initial calculation model according to the epoxy sample internal temperature and the ambient temperature; A convection cooling rate fitting function determination module is used to determine a convection cooling rate fitting function according to the initial calculation model of the curing degree of the epoxy sample; An epoxy sample curing degree optimal calculation model determination module is used to calibrate the epoxy sample curing degree initial calculation model through the convection cooling rate fitting function to determine the epoxy sample curing degree optimal calculation model; The epoxy sample curing degree acquisition module is used to obtain the epoxy sample curing degree through the epoxy sample curing degree optimal calculation model.

10. A computer-readable storage medium storing a computer program, wherein when the computer program is executed by a processor, the processor is caused to perform the steps of the method according to any one of claims 1 to 8.

11. A computer device comprising a memory and a processor, wherein the memory stores a computer program, and when the computer program is executed by the processor, the processor executes the steps of the method according to any one of claims 1 to 8.

Images