A material flame retardant performance testing device and method used in conjunction with a spectrometer

Abstract

The invention belongs to the technical field of material flame retardant performance testing, and discloses a material flame retardant performance testing device and method used in conjunction with a spectrometer, comprising a collection box; the collection box is in the shape of a sealed box with a hollow interior, a through hole groove is provided on any side wall of the collection box, and a covering component for covering the sample surface is provided on the outer side wall of the collection box where the through hole groove is provided, and the covering component is arranged around the through hole groove; a spark flashing mechanism is provided on the collection box, and the spark flashing mechanism is used to generate sparks for burning the sample surface at the through hole groove; an optical fiber is fixedly connected to one end of the collection box away from the through hole groove, and the other end of the optical fiber is used to connect to a spectrometer, and the optical fiber is used to guide the excitation light of the spectrometer to the sample surface and transmit the spectral signal of the sample to the spectrometer; the flame retardant performance of the sample is judged by analyzing the change of the spectral signal of the sample before and after burning, and because the enclosed space limits the oxygen supply, it can effectively prevent the sample from being continuously burned, and avoid structural damage to the sample.

Description

Technical Field

[0001] The invention belongs to the technical field of material flame retardancy testing, and in particular relates to a material flame retardancy testing device and method used in conjunction with a spectrometer. Background Art

[0002] With the continuous development of science and technology, the existing material combustion performance testing equipment, such as cone calorimeter, horizontal vertical combustion tester and various combustion test machines, all have the same testing principle: the test sample is made into a sample of specified size and placed in a flame environment to observe or calculate the combustion oxygen consumption, combustion heat release, flame extinction speed and other combustion state information of the sample; for example, Chinese patent CN 119224048 A discloses a flame retardant performance testing device for environmentally friendly, highly weather-resistant, flame-retardant ABS plastics, which is mainly used to test the flame retardant performance of plastics under different environmental conditions. Its working principle includes accurately adjusting the distance between the sample to be tested and the flamethrower through a clamping component to ensure the standardization of the combustion test. The device is equipped with a combustion component, a detection component and a temperature and gas control component, which can monitor the temperature, gas composition and combustion state in real time; the smoke filter component effectively treats the harmful gases generated by combustion to ensure the safety of the experimental environment; its advantage is that it has strong applicability and can simulate a variety of environmental conditions and improve the detection accuracy; its disadvantage is that the sample is burned by flames during the test, and the test process causes irreversible damage to the sample. The test process is destructive. After the flame retardant performance test, the sample cannot be used anymore regardless of whether it is burned or not; therefore, there is a problem in the prior art that the sample is easily structurally damaged during the test, resulting in the sample being unable to be used anymore. Summary of the invention

[0003] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a material flame retardancy testing device and method for use with a spectrometer, which solves the problem in the prior art that structural damage is easily caused to the sample during the test, resulting in the sample being unable to continue to be used.

[0004] The purpose of the present invention can be achieved through the following technical solutions:

[0005] A material flame retardant performance testing device used in conjunction with a spectrometer, comprising a collection box;

[0006] The collection box is in the shape of a sealed box with a hollow interior. A through hole groove is provided on any side wall of the collection box. A covering component for covering the sample surface is provided on the outer side wall of the collection box where the through hole groove is provided. The covering component is arranged around the through hole groove.

[0007] The collection box is provided with a spark flashing mechanism, which is used to generate sparks at the through-hole groove to burn the surface of the sample;

[0008] An optical fiber is fixedly connected to one end of the collection box away from the through-hole groove, and the other end of the optical fiber is used to connect to the spectrometer. The optical fiber is used to guide the excitation light of the spectrometer to the sample surface and transmit the spectral signal of the sample to the spectrometer;

[0009] The spark flashing mechanism comprises a spark flashing window and a spark generator, the spark generator is fixedly mounted on the collection box, the spark flashing window is fixed on the slot wall of the through hole slot, and the spark flashing window is connected to the spark generator through a wire;

[0010] The covering component includes a sealing cover, which is made of elastic material and fixed to the outer wall of the collection box on the side where the through hole groove is opened. The sealing cover and the through hole groove are coaxially placed, and both ends of the sealing cover along the axis direction of the through hole groove are open. The through hole groove is located on the inner side of the sealing cover, and the internal cross-sectional area of ​​the sealing cover gradually increases from the end close to the collection box to the end away from the collection box.

[0011] An exhaust hole is provided on any side wall of the collection box, and an air valve is provided in the exhaust hole;

[0012] The sum of the internal volume of the collection box and the internal volume of the sealing cover is less than 1000 cubic centimeters;

[0013] A method for testing the flame retardant properties of a material used in conjunction with a spectrometer, using a material flame retardant properties testing device used in conjunction with a spectrometer to test the flame retardant properties of a sample, specifically comprising the following steps:

[0014] preparing samples, the samples comprising a plurality of learning samples and test samples, wherein the learning samples are all made of materials with known flame retardant properties;

[0015] The samples are tested using a material flame retardant performance testing device used in conjunction with a spectrometer to obtain the difference spectrum data of each learning sample and the test sample before and after burning;

[0016] Based on the difference spectrum data of the learning samples, a prediction model for predicting the flame retardant properties of materials is constructed;

[0017] Using the known flame retardant properties of the learning samples as labels, machine learning technology is used to learn and train the prediction model;

[0018] The difference spectrum data of the test sample is input into the prediction model, and the flame retardant performance of the test sample is output;

[0019] The samples are tested using a material flame retardant performance testing device used in conjunction with a spectrometer to obtain the difference spectrum data of each learning sample and the test sample before and after burning, specifically including the following steps:

[0020] Determine the position of the sample to be tested, wipe and clean the position of the sample to be tested with cleaning liquid, and let the sample stand and dry;

[0021] Connect the optical fiber to the spectrometer;

[0022] Covering the covering component on the position of the sample to be tested;

[0023] Turn on the spectrometer to obtain the spectrum signal of the sample surface before burning;

[0024] Turn on the spark flashing mechanism to generate sparks to burn the sample surface;

[0025] Turn on the spectrometer again to obtain the spectral signal of the sample surface after burning;

[0026] Compare the spectral signals obtained before and after burning to obtain the difference spectrum data of each learning sample and the test sample before and after burning;

[0027] The spark flash mechanism generates sparks with a heat energy range of 10-5000 joules, and the time for the spark to burn the sample surface is less than 10 seconds;

[0028] The cleaning solution includes one or more of alcohol, pure water, acetone, carbon tetrachloride, and ethyl acetate;

[0029] The machine learning techniques include one or more of extreme gradient descent XGBoost, support vector machine SVM, random forest, and Bayesian optimization extreme gradient descent BO-XGBoost.

[0030] Beneficial effects of the present invention:

[0031] The present invention covers the position of the sample to be tested by a covering component, so that the collection box and the position of the sample to be tested form a closed space, and sparks are generated by a spark flashing mechanism to burn the surface of the sample. At the same time, the spectral signals of the sample before and after burning are collected by a spectrometer, and the flame retardant performance of the sample is judged by analyzing the changes in the spectral signals of the sample before and after burning. Since the closed space limits the oxygen supply, it can effectively prevent the sample from being continuously burned, avoiding structural damage to the sample. At the same time, the present application is suitable for flame retardant performance testing of materials of different sizes. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] 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, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0033] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0034] Figure 2 It is a schematic diagram of the overall structure of the present invention from different viewing angles;

[0035] Figure 3 It is a schematic diagram of the spark flashing mechanism structure of the present invention;

[0036] Figure 4 It is a schematic flow chart of the material flame retardancy testing method of the present invention;

[0037] Figure 5 It is the spectrum signal diagram of the sample of the present invention before and after spark burning;

[0038] Figure 6 It is a schematic diagram of the difference spectrum data of the sample of the present invention before and after spark burning. DETAILED DESCRIPTION

[0039] 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.

[0040] like Figures 1 to 6 As shown, a material flame retardant performance testing device used in conjunction with a spectrometer includes a collection box 4;

[0041] The collection box 4 is in the shape of a sealed box with a hollow interior. A through hole 41 is provided on any side wall of the collection box 4. A covering component 1 for covering the sample surface is provided on the outer side wall of the collection box 4 at the end where the through hole 41 is provided. The covering component 1 is arranged around the through hole 41.

[0042] The collection box 4 is provided with a spark flashing mechanism 3, and the spark flashing mechanism 3 is used to generate sparks at the through hole groove 41 to burn the surface of the sample;

[0043] An optical fiber 5 is fixedly connected to one end of the collection box 4 away from the through hole 41, and the other end of the optical fiber 5 is used to connect to the spectrometer. The optical fiber 5 is used to guide the excitation light of the spectrometer to the sample surface and transmit the spectral signal of the sample to the spectrometer;

[0044] The present application covers the sample by a covering component 1, so that a closed space is formed in the covering component 1 and the collection box 4, and the spectrum signal of the sample before burning is collected by a spectrometer, and then the spark flashing mechanism 3 is turned on to generate sparks to burn the surface of the sample. Since the closed space limits the oxygen supply, it can effectively prevent the sample from being continuously burned and avoid structural damage to the sample. After the burning is completed, the sample spectrum signal is collected by the spectrometer, and the flame retardant performance of the sample is judged by analyzing the change characteristics of the sample spectrum signal before and after burning.

[0045] Preferably, the spectrometer can be an infrared or Raman spectrometer, which guides the excitation light of the spectrometer to the sample, and transmits the absorption, refraction and reflection results of the excitation light to the spectrometer for analysis. The flame retardant properties of the material can be judged by detecting the generated gas, smoke or other chemicals and based on these changes.

[0046] The spark flashing mechanism 3 generates sparks with a heat energy range of 10-5000 joules, and the time for the spark to burn the sample surface is less than 10 seconds; so that the generated sparks can burn the sample surface without causing structural damage to the sample;

[0047] According to research and experiments, for samples with flame retardancy reaching V0 level, in a closed space of 1000 cubic centimeters, heat energy within 5000 joules will not cause significant changes in the chemical composition and surface morphology of the samples; for samples with flame retardancy below V0, heat energy above 10 joules acting on the samples can produce changes in chemical composition and chemical environment sufficient to be detected by conventional spectrometers.

[0048] The spark flashing mechanism 3 includes a spark flashing window 31 and a spark generator 32. The spark generator 32 is fixedly mounted on the collection box 4. The spark flashing window 31 is fixed on the groove wall of the through hole groove 41. The spark flashing window 31 is connected to the spark generator 32 through a wire. The spark generator 32 generates high voltage current by pressing piezoelectric ceramics or an external power supply. The current reaches the spark flashing window 31 along the wire and generates flashing sparks under the action of the voltage difference. The spark acts on the sample surface to produce controllable ablation, causing changes in the chemical composition of the sample surface material.

[0049] The covering component 1 includes a sealing cover, which is made of an elastic material and is fixed to the outer wall of the collection box 4 on the side where the through hole groove 41 is opened. The sealing cover and the through hole groove 41 are placed coaxially, and both ends of the sealing cover along the axial direction of the through hole groove 41 are open. The through hole groove 41 is located on the inner side of the sealing cover, and the internal cross-sectional area of ​​the sealing cover gradually increases from the end close to the collection box 4 to the end away from the collection box 4.

[0050] An exhaust hole is provided on any side wall of the collection box 4, and an air valve 2 is provided in the exhaust hole;

[0051] It should be noted that this application is applicable to the flame retardant performance testing of various types of materials, such as rubber, plastic, organic materials, inorganic materials and composite materials, and this application can also be applied to the testing of samples of various sizes;

[0052] Preferably, the sealing cover can be made of elastic rubber material;

[0053] For samples of materials with smooth surfaces, the sealing cover can be directly attached to the surface of the material to form a closed space required for airtight testing;

[0054] For samples of materials with rough surfaces, when testing such materials, it is necessary to prepare samples with a size smaller than the cross-section size of the sealing cover away from the 4 ends of the collection box, and use them with a bearing plane with a smooth surface. The bearing plane can be made of stainless steel, hard fireproof board, heat-resistant ceramic board, etc. Place the sample on the bearing plane, and then attach the sealing cover to the bearing plane to form a sealed space required for testing;

[0055] For samples whose size is smaller than the cross-section of the sealing cover away from the collection box, a bearing plane must be used regardless of whether the surface of the material is smooth.

[0056] Before the sealing cover contacts the sample surface or the carrying plane, the air valve 2 is opened first, and then the sealing cover is pushed to contact with the sample surface to squeeze and compress the sealing cover. After the squeezing and compression are completed, the air valve 2 is closed, so that the sealing cover is tightly adsorbed on the sample surface or the carrying plane, and at the same time, a closed space is formed between the sealing cover and the collection box 4 to limit the oxygen supply and prevent the sample from continuing to burn;

[0057] At the same time, the sealing cover covers the detection position of the sample to prevent the ambient light from interfering with the collection of spectral signals.

[0058] The sum of the internal volume of the collection box 4 and the internal volume of the sealing cover is less than 1000 cubic centimeters; the oxygen content in the sealed space formed after the sealing cover is adsorbed with the sample or the supporting plane is effectively limited, so that the sample undergoes controllable instantaneous burning under the action of the spark without significant and continuous combustion, thereby avoiding combustion damage to the sample.

[0059] like Figure 4 As shown, a method for testing the flame retardant properties of materials used in conjunction with a spectrometer is used to test the flame retardant properties of a sample using a material flame retardant properties testing device used in conjunction with a spectrometer, and specifically includes the following steps:

[0060] preparing samples, the samples comprising a plurality of learning samples and test samples, wherein the learning samples are all made of materials with known flame retardant properties;

[0061] The samples are tested using a material flame retardant performance testing device used in conjunction with a spectrometer to obtain the difference spectrum data of each learning sample and the test sample before and after burning;

[0062] Based on the difference spectrum data of the learning samples, a prediction model for predicting the flame retardant properties of materials is constructed;

[0063] Using the known flame retardant properties of the learning samples as labels, machine learning technology is used to learn and train the prediction model;

[0064] The difference spectrum data of the test sample is input into the prediction model, and the flame retardant performance of the test sample is output;

[0065] The samples are tested using a material flame retardant performance testing device used in conjunction with a spectrometer to obtain the difference spectrum data of each learning sample and the test sample before and after burning, specifically including the following steps:

[0066] Determine the position of the sample to be tested, wipe and clean the position of the sample to be tested with cleaning liquid, and let the sample stand and dry;

[0067] Connect the end of the optical fiber 5 away from the collection box 4 to the spectrometer;

[0068] Covering the covering component 1 on the position of the sample to be tested;

[0069] Turn on the spectrometer to obtain the spectrum signal of the sample surface before burning;

[0070] Turn on the spark flashing mechanism 3 to generate sparks to burn the surface of the sample;

[0071] Turn on the spectrometer again to obtain the spectral signal of the sample surface after burning;

[0072] Compare the spectral signals obtained before and after burning to obtain the difference spectrum data of each learning sample and the test sample before and after burning;

[0073] The cleaning solution includes one or more of alcohol, pure water, acetone, carbon tetrachloride, and ethyl acetate;

[0074] The machine learning techniques include one or more of extreme gradient descent XGBoost, support vector machine SVM, random forest, and Bayesian optimization extreme gradient descent BO-XGBoost.

[0075] In this application, samples made of polycarbonate composite materials were used to verify the prediction model;

[0076] During the verification process, alcohol is used to wipe and clean the location to be tested;

[0077] During the verification process, a mobile Raman spectrometer (ReactRaman 802L, METTLER) was selected to connect to optical fiber 5;

[0078] During the verification process, a spark with a heat energy of 2000 joules and a burning time of 2 seconds was used;

[0079] During the verification process, 10 samples were prepared and numbered from 1 to 10. Sample 10 was selected as the test sample and samples 1 to 9 were selected as the learning samples. The spectral signals of samples 1 to 10 before and after burning are shown in Figure 2. Figure 5 As shown, the difference spectrum data of samples 1-10 before and after burning are as follows Figure 6 As shown;

[0080] Based on the difference spectrum data obtained from samples 1-9, the prediction models were trained using four machine learning techniques respectively. The accuracy, precision, recall and F1 scores of the training results of the four machine learning techniques are shown in Table 1. The Raman difference spectrum of the test sample was analyzed using the BO-XGBoost model with the best accuracy, and it was found that the flame retardant performance of sample 10 was V0 level.

[0081] Table 1. Training results of four machine learning techniques

[0082]

[0083] By conducting a combustion performance test on the samples, it was also found that the flame retardant performance of sample 10 was V0 level, which further verified the accuracy and feasibility of the test of this application.

[0084] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0085] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited by the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.

Claims

1. A material flame retardancy testing device used in conjunction with a spectrometer, comprising a collection box (4), characterized in that: The collection box (4) is in the shape of a sealed box with a hollow interior. A through hole groove (41) is provided on any side wall of the collection box (4). A covering component (1) for covering the surface of the sample is provided on the outer side wall of the collection box (4) at the end where the through hole groove (41) is provided. The covering component (1) is arranged around the through hole groove (41). A spark flashing mechanism (3) is provided on the collection box (4), and the spark flashing mechanism (3) is used to generate sparks at the through hole groove (41) to burn the surface of the sample; An optical fiber (5) is fixedly connected to one end of the collection box (4) away from the through hole groove (41), and the other end of the optical fiber (5) is used to connect to a spectrometer. The optical fiber (5) is used to guide the excitation light of the spectrometer to the sample surface and transmit the spectral signal of the sample to the spectrometer; The covering component (1) comprises a sealing cover, the sealing cover is made of an elastic material, the sealing cover is fixed to the outer wall of the collection box (4) on the side where the through hole groove (41) is provided, the sealing cover and the through hole groove (41) are coaxially arranged, both ends of the sealing cover along the axis direction of the through hole groove (41) are open, the through hole groove (41) is located on the inner side of the sealing cover, and the internal cross-sectional area of ​​the sealing cover gradually increases from the end close to the collection box (4) to the end away from the collection box (4); An exhaust hole is provided on any side wall of the collection box (4), and an air valve (2) is provided in the exhaust hole; The sum of the internal volume of the collection box (4) and the internal volume of the sealing cover is less than 1000 cubic centimeters; The spark flashing mechanism (3) generates a spark with a heat energy range of 10-5000 joules, and the time for the spark to burn the sample surface is less than 10 seconds.

2. The material flame retardancy testing device used in conjunction with a spectrometer according to claim 1, characterized in that: The spark flicker mechanism (3) comprises a spark flicker window (31) and a spark generator (32). The spark generator (32) is fixedly mounted on the collection box (4). The spark flicker window (31) is fixed on the groove wall of the through hole groove (41). The spark flicker window (31) is connected to the spark generator (32) via a wire.

3. A method for testing the flame retardant properties of materials used in conjunction with a spectrometer, using the flame retardant properties testing device for materials used in conjunction with a spectrometer as described in any one of claims 1-2 to test the flame retardant properties of a sample, characterized in that: The specific steps include: preparing samples, the samples comprising a plurality of learning samples and test samples, wherein the learning samples are all made of materials with known flame retardant properties; The samples are tested using a material flame retardant performance testing device used in conjunction with a spectrometer to obtain the difference spectrum data of each learning sample and the test sample before and after burning; Based on the difference spectrum data of the learning samples, a prediction model for predicting the flame retardant properties of materials is constructed; Using the known flame retardant properties of the learning samples as labels, machine learning technology is used to learn and train the prediction model; The difference spectrum data of the test sample is input into the prediction model, and the flame retardant performance of the test sample is output.

4. The material flame retardancy testing method for use with a spectrometer according to claim 3, characterized in that: The samples are tested using a material flame retardant performance testing device used in conjunction with a spectrometer to obtain the difference spectrum data of each learning sample and the test sample before and after burning, specifically including the following steps: Determine the position of the sample to be tested, wipe and clean the position of the sample to be tested with cleaning liquid, and let the sample stand and dry; Connecting the optical fiber (5) to the spectrometer; Covering the covering component (1) on the position of the sample to be tested; Turn on the spectrometer to obtain the spectrum signal of the sample surface before burning; Turning on the spark flashing mechanism (3) to generate sparks to burn the surface of the sample; Turn on the spectrometer again to obtain the spectral signal of the sample surface after burning; The spectral signals obtained before and after burning are compared to obtain the difference spectrum data of each learning sample and test sample before and after burning.

5. The material flame retardancy testing method for use with a spectrometer according to claim 4, characterized in that: The cleaning solution includes one or more of alcohol, pure water, acetone, carbon tetrachloride, and ethyl acetate.

6. The material flame retardancy testing method for use with a spectrometer according to claim 5, characterized in that: The machine learning techniques include one or more of extreme gradient descent XGBoost, support vector machine SVM, random forest, and Bayesian optimization extreme gradient descent BO-XGBoost.

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