CN113030167A - Silicone rubber material aging state fine evaluation method based on TGA-FTIR - Google Patents
Silicone rubber material aging state fine evaluation method based on TGA-FTIR Download PDFInfo
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 60
- 238000000003 thermogravimetry coupled to Fourier transform infrared spectroscopy Methods 0.000 title claims abstract description 30
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 22
- 238000011156 evaluation Methods 0.000 title claims abstract description 8
- 238000004643 material aging Methods 0.000 title abstract description 4
- 238000012360 testing method Methods 0.000 claims abstract description 144
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims abstract description 50
- 239000000463 material Substances 0.000 claims abstract description 45
- 230000032683 aging Effects 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000005259 measurement Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 230000008859 change Effects 0.000 claims description 10
- 238000002474 experimental method Methods 0.000 claims description 10
- 238000002835 absorbance Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000428 dust Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 6
- 238000001303 quality assessment method Methods 0.000 claims 9
- 238000013441 quality evaluation Methods 0.000 abstract description 2
- 238000002411 thermogravimetry Methods 0.000 description 45
- 239000002131 composite material Substances 0.000 description 10
- 239000012212 insulator Substances 0.000 description 10
- 229920001971 elastomer Polymers 0.000 description 6
- 230000036962 time dependent Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- -1 polymethylvinylsiloxane Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a TGA-FTIR-based silicone rubber material aging state fine evaluation method, which comprises the following steps of 1, preparing a sample, and selecting a silicone rubber material after operation as a test sample; 2, connecting an FTIR experimental instrument gas measuring unit with a TGA test unit, and testing parameters; 3 the samples are respectively subjected to TGA-FTIR test; 4, drawing a characteristic curve; 5, evaluating the aging degree. The invention defines the test flow and the judgment basis of the TGA-FTIR of the silicon rubber material, and provides a new reference for the quality evaluation and the residual life prediction of the silicon rubber material.
Description
Technical Field
The invention belongs to the technical field of silicon rubber material performance research, and particularly relates to a TGA-FTIR-based method for finely evaluating the aging state of a silicon rubber material.
Background
Silicon rubber materials are widely favored by power enterprises due to excellent pollution flashover resistance, and the application amount of the silicon rubber materials (high-temperature vulcanized silicon rubber composite insulators and normal-temperature vulcanized silicon rubber pollution flashover resistant coatings (RTV)) in power systems is increased explosively after large-area pollution flashover accidents in China at the beginning of the century since the end of the last century. By far, the net hanging amount of the composite insulator in China breaks through 900 ten thousand, and the RTV basically realizes that the composite insulator is required to be painted when meeting porcelain.
However, when the silicone rubber material is used as an organic polymer material, the running state of the silicone rubber material inevitably undergoes degradation, i.e., aging, due to the combined action of factors such as a strong electric field, ultraviolet rays, high temperature, oxygen, dirt, moisture and the like during the operation of the suspended net. Therefore, research institutions and scholars at home and abroad carry out a great deal of research on the aging characteristic of the silicon rubber material, and propose that the aging state of the silicon rubber is represented by the performance of the base rubber (polymethylvinylsiloxane), and the physical, chemical and electrical characteristics of the base rubber are analyzed through Thermal Gravimetric Analysis (TGA), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscope (SEM), Thermal Stimulation Current (TSC), X-ray photoelectron spectroscopy (XPS) and the like. However, the silicon rubber material is a mixture formed by vulcanizing base rubber and various organic and inorganic fillers at high temperature, and various performances of the base rubber and the fillers are directly crossed and overlapped to a certain extent, so that the existing silicon rubber material aging evaluation method has larger error.
Therefore, a new method for evaluating the aging state of the silicone rubber material is urgently needed on the basis of analyzing and testing various performances of the base rubber and the filler, the base rubber and the filler are distinguished, the fine evaluation of the aging of the silicone rubber material is realized, so that a power enterprise is guided to formulate a rotation strategy of the composite insulator and the RTV anti-pollution flashover coating, the safe and reliable operation of power equipment is guaranteed, and the repeated investment of the power equipment is reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for finely evaluating the aging state of a silicon rubber material based on TGA-FTIR.
The technical scheme adopted by the invention for solving the technical problems is as follows:
which comprises the following steps of,
(1) preparing a sample, namely selecting a silicon rubber material after operation as a test sample;
(2) connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
(3) the samples were subjected to TGA-FTIR testing, respectively;
(4) drawing a characteristic curve;
(5) and (5) evaluating the aging degree.
Further, in the step (1), samples are cut from the operated silicon rubber material, the contact surface of the samples with air is completely preserved in the operation process, the weight of the samples is 20mg +/-3 mg, and the thickness of the samples is not more than 1 mm.
Further, in the step (1), the surface of the test sample is wiped off by absolute ethyl alcohol, and then the test sample is placed in a dust cover to be naturally dried.
Further, in step (2), connecting the FTIR laboratory gas measuring unit with the TGA testing unit; the measurement interval of the FTIR test is set to be not less than 1 time/s.
Further, in the step (2), a heating device is arranged at a connecting pipeline between the FTIR tester gas measurement unit and the TGA test tail gas discharge port, and the FTIR tester gas measurement unit and the TGA test tail gas discharge port are automatically insulated when heated to at least 200 ℃.
Further, in the step (2), the TGA test atmosphere is set to be nitrogen, the gas flow rate is 40-70ml/min, the test minimum temperature is set to be 20-30 ℃, the test maximum temperature is 750-.
Further, in the step (3), the test sample is placed in a TGA experimental instrument, the weight of the test sample is recorded as M, the sample is clamped by using clean tweezers in the moving process, and the sample is prevented from being touched by hands;
when the TGA experimental device reaches the lowest temperature of the experiment and the nitrogen gas is introduced for no less than 30min, the TGA and FTIR experiments are started simultaneously.
Further, in the step (4), drawing a characteristic curve; after the experiment is finished, the wave number in single test data of FTIR is selected to be 2960 +/-15 cm-1And drawing a time-dependent change curve of the characteristic quantity by taking the maximum value of the medium absorbance peak as the characteristic quantity N, taking the characteristic quantity as a Y axis and taking the test time as an X axis.
Further, in the step (5), the evaluation method is as follows:
and integrating the change curve of the characteristic quantity N along with the test time to obtain an area S enclosed by the curve and the coordinate axis, and further obtain a normalized value K = S/M of the S. Wherein M is the weight M recorded in the step (3).
Further, the K value is inversely proportional to the aging degree of the silicon rubber material.
The invention has the beneficial effects that:
(1) the wave number of methane which is a unique decomposition product of the silicon rubber material is 2960±15cm-1The absorbance in the range represents the hydrophobic endurance performance of the silicone rubber material, and further represents the aging degree of the silicone rubber material.
(2) According to the invention, the aging degree of the silicon rubber material is represented by the content of the special decomposition product of the silicon rubber material, so that the accuracy of the aging evaluation of the silicon rubber material is improved.
(3) The invention defines the test flow and the judgment basis of the TGA-FTIR of the silicon rubber material, and provides a new reference for the quality evaluation and the residual life prediction of the silicon rubber material.
(4) According to the method, the content of organic matters in the silicone rubber material under unit mass is obtained through normalization treatment, and the influence of the weight, the area and the like of the silicone rubber material on the result is eliminated.
Drawings
FIG. 1 is a schematic block diagram of the connection of a TGA-FTIR testing apparatus;
FIG. 2 is a flow chart of the present invention;
figure 31 # sample TGA-FTIR test profile;
figure 42 # sample TGA-FTIR test profile;
figure 53 # sample TGA-FTIR test profile.
Detailed Description
The present invention is further described in detail below with reference to examples, but the scope of the present invention is not limited thereto, and the scope of the invention is set forth in the claims.
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the application, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Example 1
As shown in fig. 1 to 5, the present invention includes the steps of,
(1) preparing a sample, namely selecting a silicon rubber material after operation as a test sample; samples are cut from the operated silicon rubber material, the contact surface of the samples with air is completely preserved in the operation process, the weight of the samples is 20mg +/-3 mg, and the thickness of the samples is not more than 1 mm. And wiping the surface of the test sample with absolute ethyl alcohol to remove dirt, and then placing the test sample in a dust cover to naturally dry.
(2) Connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
(3) the samples were subjected to TGA-FTIR testing, respectively;
(4) drawing a characteristic curve;
(5) and (5) evaluating the aging degree.
The specific operation is as follows:
(1) selecting 3 running composite insulators, cutting silicon rubber samples with similar shapes and sizes on the upper surface of the umbrella skirt of the high-voltage end of the composite insulators by using a wallpaper cutter, and completely preserving the upper surfaces of the samples without damage and electric erosion, wherein the samples are respectively numbered as 1#, 2#, and 3 #.
The surface of the test sample is wiped off with absolute ethyl alcohol, and then the test sample is placed in a dust cover to be naturally dried for 2 hours in the embodiment.
(2) Connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
the gas measuring unit of the FTIR experimental instrument is connected with the TGA testing unit, the schematic connection diagram is shown in fig. 1, the measuring unit of the fourier transform infrared spectrometer and the thermogravimetric analyzer are connected by a testing unit connecting pipeline, the connection mode is known by those skilled in the art, that is, the gas outlet of the thermogravimetric analyzer is connected with the testing gas inlet of the FTIR experimental instrument, so as to realize the connection of the two devices.
In which the water bath system acts directly on the thermo-gravimetric analyzer (TGA). The computer can control the FTIR laboratory instrument and the thermogravimetric analyzer (TGA) at the same time.
After a gas measurement unit of the FTIR experimental instrument is connected with a TGA test unit, the whole device is replaced by nitrogen and continuously filled with nitrogen, and then test parameters are set;
in the step (2), connecting an FTIR experimental instrument gas measuring unit with a TGA test unit; FTIR test measurements were set at 4 time/s intervals.
In the step (2), setting the TGA test atmosphere as nitrogen, setting the gas flow rate as 40ml/min, setting the test minimum temperature as 30 ℃, the test maximum temperature as 780 ℃, and setting the heating rate as 20 ℃/min.
In the step (2), a heating device is arranged at a connecting pipeline between the gas measurement unit of the FTIR tester and a tail gas discharge port of the TGA test, and the heating device is heated to 260 ℃ and then automatically keeps the temperature.
(3) The samples were subjected to TGA-FTIR testing, respectively;
in the step (3), a test sample is placed in a TGA experimental instrument, the weight of the test sample is recorded as M, the sample is clamped by using clean tweezers in the moving process, and the sample is forbidden to touch by hands; specifically, three silicone rubber samples were placed in a TGA test furnace with tweezers to obtain the weight M1=19.569mg、M2=20.807mg、M3=20.814mg, FTIR test started.
When the TGA experimental device reaches the lowest temperature of the experiment and the nitrogen gas is introduced for no less than 30min, the TGA and FTIR experiments are started simultaneously.
In the step (4), drawing a characteristic curve; selecting FTIR single test data with wave number of 2960 +/-15 cm-1And drawing a time-dependent change curve of the characteristic quantity by taking the maximum value of the medium absorbance peak as the characteristic quantity N, taking the characteristic quantity as a Y axis and taking the test time as an X axis.
After the test is finished, three samples are selected, and the wave number in each FTIR test result is 2960 +/-15 cm-1The maximum value of absorbance in the range is a characteristic quantity N, the N value is taken as a Y axis, the test temperature is taken as an X axis, and a change curve L of the N along with the test temperature is drawn1、L2、L3As shown in fig. 3-5.
To LxIntegrating at an integration temperature range of 30-800 deg.C to obtain curve LxThe areas of the city enclosed by the coordinate axes are respectively recorded as S1=6.366、S2=4.320、S3=3.973。
Normalizing to obtain KxValue, Kx=Sx/MxX is 1, 2, 3 respectively to obtain K1=0.325，K2=0.208，K3=0.191。
K3＜K2＜K1Therefore, with the increase of operation, the 3# sample is most seriously aged, and the content of the organic components in the sample is reduced to the greatest extent; the second sample was aged with a moderate decrease in the organic content, the second sample was aged with the lightest organic content, and the third sample was aged with the lightest decrease in the organic content.
Example 2
Which comprises the following steps of,
(1) preparing a sample, namely selecting a silicon rubber material after operation as a test sample; in the step (1), a sample is cut from the operated silicon rubber material, the contact surface of the sample with air is completely preserved in the operation process, the weight of the sample is 20mg +/-3 mg, and the thickness of the sample is not more than 1 mm.
And wiping the surface of the test sample with absolute ethyl alcohol to remove dirt, and then placing the test sample in a dust cover to naturally dry.
(2) Connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
(3) the samples were subjected to TGA-FTIR testing, respectively;
(4) drawing a characteristic curve;
(5) and (5) evaluating the aging degree.
The specific operation is as follows:
(1) selecting 3 running composite insulators, cutting silicon rubber samples with similar shapes and sizes on the upper surface of the umbrella skirt of the high-voltage end of the composite insulators by using a wallpaper cutter, and completely preserving the upper surfaces of the samples without damage and electric erosion, wherein the samples are respectively numbered as 4#, 5#, and 6 #.
And wiping off dirt on the surface of the test sample by using absolute ethyl alcohol, then placing the test sample in a dust cover for naturally drying, and drying for 2 hours.
(2) Connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
in the step (2), connecting an FTIR experimental instrument gas measuring unit with a TGA test unit; FTIR test measurement intervals were set at 2/s.
In the step (2), the TGA test atmosphere is set to be nitrogen, the gas flow rate is 50ml/min, the test lowest temperature is set to be 20 ℃, the test highest temperature is set to be 750 ℃, and the temperature rise rate is 30 ℃/min.
In the step (2), a gas measurement unit of the FTIR tester is connected with a tail gas discharge port of the TGA test, a heating device is arranged in a connecting pipeline, the gas measurement unit of the FTIR tester is heated to the temperature, and then the temperature is automatically kept at 200 ℃.
(3) The samples were subjected to TGA-FTIR testing, respectively;
placing the test sample in a TGA laboratory instrument, and recording the weight of the test sample as M;
the TGA test was started and the FTIR test was started when the TGA tester reached the specified test temperature and the nitrogen gas was let in for no less than 30 min.
Starting the TGA test, after 30min and when the TGA test temperature reaches the lowest test temperature of 20 ℃ and the nitrogen gas is introduced for no less than 30min, putting three silicon rubber samples into a TGA test furnace body by using tweezers to obtain the weight M of the silicon rubber samples4、M5、M6The experiment was continued and FTIR testing was started.
In the step (4), drawing a characteristic curve; selecting the wave number in FTIR test data as 2960 +/-15 cm-1And drawing a time-dependent change curve of the characteristic quantity by taking the maximum value of the medium absorbance peak as the characteristic quantity N, taking the characteristic quantity as a Y axis and taking the test time as an X axis.
After the test is finished, three samples are selected, and the wave number in each FTIR test result is 2960 +/-15 cm-1The maximum value of absorbance in the range is a characteristic quantity N, the N value is taken as a Y axis, the test temperature is taken as an X axis, and a change curve L of the N along with the test temperature is drawn4、L5、L6。
To LxIntegrating at an integration temperature range of 30-800 deg.C to obtain curve LxThe areas of the city enclosed by the coordinate axes are respectively recorded as S4、S5、S6。
Normalizing to obtain KxValue, Kx=Sx/MxX is 4, 5, 6 respectively to obtain K4，K5，K6。
K6＜K5＜K4Therefore, the 6# sample is most seriously aged and the content of the organic components in the sample is reduced to the greatest extent along with the increase of the running; the second sample was aged to a moderate degree with a moderate reduction in the organic content, the second sample was aged the least and the second sample was aged the least with a minimal reduction in the organic content.
Example 3
Which comprises the following steps of,
(1) preparing a sample, namely selecting a silicon rubber material after operation as a test sample; in the step (1), the weight of the sample is 20mg +/-3 mg, the contact surface of the sample with air is completely preserved in the running process, and the thickness of the sample is not more than 1 mm. And wiping the surface of the test sample with absolute ethyl alcohol to remove dirt, and then placing the test sample in a dust cover to naturally dry.
(2) Connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
(3) the samples were subjected to TGA-FTIR testing, respectively;
(4) drawing a characteristic curve;
(5) and (5) evaluating the aging degree.
The specific operation is as follows:
(1) selecting 3 running composite insulators, cutting silicon rubber samples with similar shapes and sizes on the upper surface of the umbrella skirt of the high-voltage end of the composite insulators by using a wallpaper cutter, and completely preserving the upper surfaces of the samples without damage and electric erosion, wherein the samples are respectively numbered as 7#, 8#, and 9 #.
And (3) wiping the surface of the test sample with absolute ethyl alcohol to remove dirt, then placing the test sample in a dust cover to naturally dry, and drying for 2 hours.
(2) Connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
in the step (2), connecting an FTIR experimental instrument gas measuring unit with a TGA test unit; FTIR test measurement intervals were set at 1 time/s.
In the step (2), the TGA test atmosphere is set to be nitrogen, the gas flow rate is 70ml/min, the test minimum temperature is set to be 25 ℃, the test maximum temperature is set to be 800 ℃, and the temperature rise rate is 10 ℃/min.
In the step (2), a gas measurement unit of the FTIR tester is connected with a tail gas discharge port of the TGA test, a heating device is arranged in a connecting pipeline, the gas measurement unit of the FTIR tester is heated to the temperature, and then the temperature is automatically kept at 210 ℃.
(3) The samples were subjected to TGA-FTIR testing, respectively;
placing the test sample in a TGA laboratory instrument, and recording the weight of the test sample as M;
the TGA test was started, and the FTIR test was started when the TGA tester reached 25 ℃ and nitrogen was passed for no less than 30 min.
Starting the TGA test, after 30min and when the TGA test temperature reaches 25 ℃ and the nitrogen gas introduction time is not less than 30min, putting three silicon rubber samples into a TGA test furnace body by using tweezers to obtain the weight M of the silicon rubber samples7、M8、M9The experiment was continued and FTIR testing was started.
In the step (4), drawing a characteristic curve; selecting the wave number in FTIR test data as 2960 +/-15 cm-1And drawing a time-dependent change curve of the characteristic quantity by taking the maximum value of the medium absorbance peak as the characteristic quantity N, taking the characteristic quantity as a Y axis and taking the test time as an X axis.
After the test is finished, three samples are selected, and the wave number in each FTIR test result is 2960 +/-15 cm-1The maximum value of absorbance in the range is a characteristic quantity N, the N value is taken as a Y axis, the test temperature is taken as an X axis, and a change curve L of the N along with the test temperature is drawn7、L8、L9。
To LxIntegrating at an integration temperature range of 30-800 deg.C to obtain curve LxThe areas of the city enclosed by the coordinate axes are respectively recorded as S7、S8、S9。
Normalizing to obtain KxValue, Kx=Sx/MxX is 4, 5, 6 respectively to obtain K7，K8，K9。
K9＜K7＜K6Therefore, with the increase of the operation, the 9# sample is most seriously aged, and the content of the organic components in the sample is reduced to the greatest extent; the 7# sample was aged the second, with a moderate decrease in its internal organic content, the 6# sample was aged the least and with the least decrease in its internal organic content.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention
In the examples. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for finely evaluating the aging state of a silicon rubber material based on TGA-FTIR is characterized by comprising the following steps: which comprises the following steps of,
(1) preparing a sample, namely selecting a silicon rubber material after operation as a test sample;
(2) connecting a gas measuring unit of the FTIR experimental instrument with a TGA test unit and setting test parameters;
(3) the samples were subjected to TGA-FTIR testing, respectively;
(4) drawing a characteristic curve;
(5) and (5) evaluating the aging degree.
2. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in the step (1), a sample is cut from the operated silicon rubber material, the contact surface of the sample with air is completely preserved in the operation process, the weight of the sample is 20mg +/-3 mg, and the thickness of the sample is not more than 1 mm.
3. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: and (3) wiping the surface of the test sample with absolute ethyl alcohol in the step (1) to remove dirt, and then placing the test sample in a dust cover to naturally dry.
4. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in the step (2), connecting an FTIR experimental instrument gas measuring unit with a TGA test unit; the measurement interval of the FTIR test is set to be not less than 1 time/s.
5. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in the step (2), a heating device is arranged at a connecting pipeline between a gas measuring unit of the FTIR test instrument and a tail gas discharge port of the TGA test, and the temperature is automatically preserved when the gas measuring unit and the tail gas discharge port are heated to at least 200 ℃.
6. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 4, wherein: in the step (2), the TGA test atmosphere is set to be nitrogen, the gas flow rate is 40-70ml/min, the test minimum temperature is set to be 20-30 ℃, the test maximum temperature is 750-.
7. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in the step (3), a test sample is placed in a TGA experimental instrument, the weight of the test sample is recorded as M, the sample is clamped by using clean tweezers in the moving process, and the sample is forbidden to touch by hands;
when the TGA experimental device reaches the lowest temperature of the experiment and the nitrogen gas is introduced for no less than 30min, the TGA and FTIR experiments are started simultaneously.
8. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in the step (4), drawing a characteristic curve; after the experiment is finished, the wave number in single test data of FTIR is selected to be 2960 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity N, the characteristic quantity is used as the Y axis, and the test time is used as the test timeAnd an X axis, and drawing a change curve of the characteristic quantity along with time.
9. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 8, wherein: in the step (5), the evaluation method comprises the following steps:
and integrating the change curve of the characteristic quantity N along with the test time to obtain an area S enclosed by the curve and the coordinate axis, and further obtain a normalized value K = S/M of the S.
10. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 9, wherein: the K value is inversely proportional to the aging degree of the silicon rubber material.
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