CN113030168A - Silicon rubber material quality evaluation method based on TGA-FTIR - Google Patents
Silicon rubber material quality evaluation method based on TGA-FTIR Download PDFInfo
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 176
- 239000000463 material Substances 0.000 title claims abstract description 98
- 238000000003 thermogravimetry coupled to Fourier transform infrared spectroscopy Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000013441 quality evaluation Methods 0.000 title claims abstract description 7
- 238000012360 testing method Methods 0.000 claims abstract description 198
- 229920001971 elastomer Polymers 0.000 claims abstract description 98
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims abstract description 77
- 238000005259 measurement Methods 0.000 claims abstract description 24
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 22
- 238000012512 characterization method Methods 0.000 claims abstract description 12
- 239000004945 silicone rubber Substances 0.000 claims description 143
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 48
- 239000007789 gas Substances 0.000 claims description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000002835 absorbance Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000003292 glue Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 238000001303 quality assessment method Methods 0.000 claims 9
- 239000000945 filler Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 40
- 239000012212 insulator Substances 0.000 description 16
- 239000002131 composite material Substances 0.000 description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
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Abstract
The invention relates to a silicon rubber material quality evaluation method based on TGA-FTIR, which comprises the following steps of 1, preparing a sample, and cutting the sample from a cured silicon rubber material and a base rubber used by the silicon rubber material; 2, connecting a gas measurement unit of the FTIR experimental instrument with a TGA test unit, and setting test parameters; 3 the samples are respectively subjected to TGA-FTIR test; 4, representing hydrophobic endurance performance; 5, calculating the content of the base rubber; 6, evaluating the quality of the silicon rubber material. According to the invention, the TGA technology and the FTIR technology are combined, so that the effective distinction of the base rubber and the filler in the silicon rubber material is realized, and the accurate characterization of the content of the base rubber in the silicon rubber material is realized.
Description
Technical Field
The invention belongs to the technical field of silicon rubber material performance research, and particularly relates to a silicon rubber material quality evaluation method based on TGA-FTIR.
Background
The silicon rubber material is widely accepted by power grid enterprises due to the excellent pollution flashover resistance, and is widely applied to power transmission lines. According to statistics, only the application amount of the silicone rubber composite insulator in China breaks through 900 thousands of the existing insulators, and the RTV anti-pollution flashover coating basically achieves 'coating when meeting porcelain'.
However, with the recent popularization of composite insulators and RTV anti-pollution flashover coating manufacturing technologies, a large number of manufacturers have made the market for silicone rubber products for electric power. Due to the difference of production processes and formulas of various manufacturers, the product quality is different, and the service life of the product of some manufacturers after being hung on a net is far from reaching the design value. The quality detection of the existing silicon rubber products mainly depends on an artificial accelerated aging test, and the existing silicon rubber products have the defects of long time consumption, complex operation, poor equivalence with a natural running environment and the like, and are difficult to popularize and apply in engineering practice. In order to prevent pollution flashover accidents and improve the operation reliability of a power grid, a power grid enterprise has to provide a regular rotation method for 8-10 years on the basis of summarizing a large amount of operation experiences, and even a rotation strategy of 'changing when stopping and changing' is provided in an extremely severe area, so that the repeated investment of the power grid is increased, the overhaul workload of personnel is heavy, white pollution to the environment after the silicon rubber product is retired is increased, and the operation reliability of the power grid is reduced.
Therefore, a quality evaluation method for the silicone rubber material is urgently needed, is applied to engineering practice, realizes quick detection of the composite insulator, optimally selects a product with the best quality, improves the economical efficiency and reliability of power grid operation, and reduces white pollution of power grid equipment rotation to the environment.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art, and provide a silicon rubber material quality evaluation method based on TGA-FTIR, so that the economical efficiency and reliability of the operation of a power grid are improved.
The technical scheme adopted by the invention for solving the technical problems is as follows:
which comprises the following steps of,
(1) preparing samples, namely cutting samples from the cured silicone rubber material and the used base rubber thereof respectively;
(2) the gas measurement unit of the FTIR experimental instrument is connected with the test unit of the TGA experimental instrument, and test parameters are set;
(3) the samples were subjected to TGA-FTIR testing, respectively;
(4) the hydrophobic endurance performance is characterized;
(5) calculating the content of the base rubber;
(6) and (4) evaluating the quality of the silicon rubber material.
Further, in step (1), the sample weight was 20. + -.3 mg.
Further, the samples cut out in the step (1) are respectively NSilicone rubberAnd NBase rubber；
And (2) further, removing dirt on the surface of the sample by using absolute ethyl alcohol in the step (1), and placing the sample in a dust cover for naturally drying.
Further, in the step (2), after the gas measurement unit of the FTIR experimental instrument is connected with the TGA test unit, the whole device is replaced by nitrogen and continuously filled with nitrogen, and then test parameters are set;
parameters for the TGA laboratory instrument were set:
the TGA experimental apparatus is in nitrogen atmosphere, the gas flow rate is not less than 40-70ml/min, and the lowest test is set
The test temperature is 20-30 ℃, the maximum test temperature is 750-800 ℃, and the heating rate is 10-20 ℃/min.
Further, in step (2), FTIR test parameters are set:
the measurement interval is not less than 1 time/s;
after the FTIR experimental instrument gas measurement unit is connected with the TGA test unit, the connecting pipeline is provided with an automatic heating device, and the temperature is automatically preserved after the gas measurement unit is heated to the temperature not lower than 200 ℃.
Further, in the step (3), the samples N are separately preparedSilicone rubberAnd NBase rubberPlaced in a TGA laboratory instrument and recorded as M in weightSilicone rubberAnd MBase rubberAnd respectively starting TGA tests, and simultaneously starting FTIR tests when the TGA test device reaches the set lowest test temperature and the nitrogen gas introduction time of the whole device is not less than 30 min.
Further, in the step (4), a sample N is selectedSilicone rubberHas a wave number of 2960 +/-15 cm in FTIR test data-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureHydrophobicityObtaining the area S of the area and the surrounding city of the abscissaHydrophobicityFurther obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialHydrophobicity=SHydrophobicity/MSilicone rubber。
Further, in the step (5), a sample N is selectedSilicone rubberAnd NBase rubberThe wave number in FTIR test data is 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber 3015、YBase glue, 3015Is drawnPreparing a curve L of the temperature change of the sample according to the test time or the test temperatureSilicone rubber、LSilicone rubberObtaining the area S of the area and the surrounding city of the abscissaSilicone rubber、SBase rubberFurther calculating the base rubber content k of the silicon rubber materialBase rubber=SSilicone rubber×MBase rubber/（SBase rubber×MSilicone rubber）。
Further, in step (6), according to kHydrophobicityAnd kBase rubberThe values were evaluated.
Further, k isHydrophobicityAnd kBase rubberThe larger the value, the better the quality of the silicone rubber material; conversely, the poorer the quality of the silicone rubber material.
The invention has the beneficial effects that:
(1) the method realizes effective distinction of the base rubber and the filler in the silicon rubber material by combining the TGA technology and the FTIR technology.
(2) The invention represents the hydrophobic lasting performance of the silicon rubber material through the content of the hydrophobic substance in the silicon rubber material, and solves the problem that the traditional method cannot represent the silicon rubber material.
(3) The invention realizes the accurate characterization of the content of the base rubber of the silicon rubber material for the first time.
(4) The invention represents the product quality of the silicon rubber material by the hydrophobic durability and the base rubber content, and reflects the aging resistance and the anti-pollution flashover capability of the silicon rubber material after aging.
Drawings
FIG. 1 TGA-FTIR sample set-up physical map;
l of Silicone rubber Material # FIG. 21Water repellency of No. 1A curve;
l of Silicone rubber Material # FIG. 31No. 1 silicone rubberA curve;
l of Silicone rubber Material # FIG. 422# Water repellencyA curve;
l of Silicone rubber Material # FIG. 522# silicon rubberA curve;
FIG. 6L of example 1 base rubberBase rubberCurve line.
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.
As shown in fig. 1-6, (1) preparing samples, and respectively cutting samples from the cured silicone rubber material and the used substrate thereof;
selecting two proportions of composite insulators produced by a certain manufacturer, and cutting off a piece of composite insulator at the umbrella skirt part of the composite insulator by using a wallpaper cutter to be used as a test silicon rubber sample NSilicone rubberRespectively recorded as 1#, 2 #. The No. 1 and the No. 2 are silicon rubber materials with different proportions and made of the same base rubber and filler. The sample weight was 20. + -.3 mg. Cutting the base rubber used by the silicon rubber material by a wallpaper cutter to be used as a test base rubber sample NBase rubber(ii) a The shape and structure of the No. 1 and No. 2 samples are similar, the samples are wiped by absolute ethyl alcohol to remove surface dirt, and the samples are placed in a dust cover to be naturally dried.
(2) And the gas measuring unit of the FTIR experimental instrument is connected with the test unit of the TGA experimental instrument, and test parameters are set.
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;
the TGA test apparatus was opened and the parameters of the TGA laboratory instrument were set:
setting the test atmosphere as nitrogen, setting the gas flow rate as 50ml/min, setting the minimum test temperature as 25 ℃, the maximum test temperature as 760 ℃ and the heating rate as 15 ℃/min.
The FTIR test device is opened, and FTIR test parameters are set:
the measurement interval was 4 times/s;
after FTIR laboratory glassware gas measurement unit is connected with TGA test unit, the connecting tube has self-heating device, begins automatic heat preservation after heating to 260 ℃, prevents gas condensation such as vapor.
(3) The samples were subjected to TGA-FTIR testing, respectively;
in the step (3), the samples N are respectively mixedSilicone rubberAnd NBase rubberPlacing in a TGA experimental instrument, and recording its weight as MSilicone rubberAnd MBase rubberAnd starting a TGA test, and simultaneously starting an FTIR test when the TGA test device reaches the lowest test temperature and the nitrogen gas is introduced into the device for not less than 30 min.
A sample of # 1 silicone rubber was placed into the TGA laboratory instrument with clean tweezers to obtain its weight, MNo. 1 silicone rubber=22.566mg, TGA test is started, FTIR test is started simultaneously when the TGA test apparatus reaches the specified test temperature and the nitrogen gas is passed for not less than 30 min. After the test is finished, respectively putting the No. 2 silicone rubber sample and the base rubber sample into a TGA experimental instrument by using clean tweezers, and repeating the test to obtain M2# silicon rubber=21.116mg，MBase rubber=20.058mg。
(4) The hydrophobic endurance performance is characterized;
selecting a sample NSilicone rubberHas a wave number of 2960 +/-15 cm in FTIR test data-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureHydrophobicityObtaining the area S of the area and the surrounding city of the abscissaHydrophobicityFurther obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialHydrophobicity=SHydrophobicity/MSilicone rubber。
FTIR test data of 1# and 2# silicon rubber materials respectively selected have wave number of 2960 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YNo. 1 Silicone rubber, 2960、Y2# Silicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureWater repellency of No. 1、L2# hydrophobicProperty of (2)Obtaining the area S of the area and the surrounding city of the abscissaWater repellency of No. 1=9.630，S2# Water repellency=7.819, and then obtaining the hydrophobic endurance quality characterization quantity k of the silicon rubber materialWater repellency of No. 1=SWater repellency of No. 1/ MNo. 1 silicone rubber=0.427，k2# Water repellency= S2# Water repellency/M2# silicon rubber=0.370。
(5) Calculating the content of the base rubber;
in the step (5), a sample N is selectedSilicone rubberAnd NBase rubberThe wave number in FTIR test data is 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureSilicone rubber、LSilicone rubberObtaining the area S of the area and the surrounding city of the abscissaSilicone rubber、SBase rubberFurther calculating the base rubber content k of the silicon rubber materialBase rubber=SSilicone rubber×MBase rubber/（SBase rubber×MSilicone rubber）。
Selected base and silicon rubber material FTIR test data has the wave number of 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity Y1# Silicone rubber, 3015、Y2# Silicone rubber, 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureNo. 1 silicone rubber、L2# silicon rubber、LBase rubberObtaining the area S of the area and the surrounding city of the abscissaNo. 1 silicone rubber=5.894，S2# silicon rubber=3.996， SBase rubber=9.452, and calculating the content k of the base rubber of the silicon rubber materialNo. 1 base rubber=SNo. 1 silicone rubber×MBase rubber/（SBase rubber×MNo. 1 silicone rubber）=55.426%；k2# base rubber=S2# silicon rubber×MBase rubber/（SBase rubber×M2# silicon rubber）=40.158%。
(6) And (4) evaluating the quality of the silicon rubber material.
And (4) evaluating the quality of the silicon rubber material. k is a radical ofWater repellency of No. 1And kNo. 1 base rubberAll values are greater than k2# Water repellencyAnd k2# base rubberAnd then, the quality of the 1# silicon rubber material is better than that of the 2# silicon rubber material.
Example 2
(1) Preparing samples, namely cutting samples from the cured silicone rubber material and the used base rubber thereof respectively;
selecting two proportions of composite insulators produced by a certain manufacturer, and cutting off a piece of composite insulator at the umbrella skirt part of the composite insulator by using a wallpaper cutter to be used as a test silicon rubber sample NSilicone rubberRespectively recorded as # 3 and # 4. 3# and 4# are silicone rubber materials with different proportions and made of the same base rubber and filler. The sample weight was 20. + -.3 mg. Cutting the base rubber used by the silicon rubber material by a wallpaper cutter to be used as a test base rubber sample NBase rubber(ii) a The shape and structure of the No. 3 and No. 4 samples are similar, the surface of the samples is wiped with absolute ethyl alcohol, and the samples are placed in a dustproof cover and naturally dried.
(2) And the gas measuring unit of the FTIR experimental instrument is connected with the test unit of the TGA experimental instrument, and test parameters are set.
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;
the TGA test apparatus was opened and the parameters of the TGA laboratory instrument were set:
setting the test atmosphere as nitrogen, the gas flow rate as 40ml/min, the test minimum temperature as 30 ℃, the test maximum temperature as 750 ℃ and the heating rate as 10 ℃/min.
The FTIR test device is opened, and FTIR test parameters are set:
the measurement interval is 1 time/s;
after FTIR laboratory glassware gas measurement unit is connected with TGA test unit, the connecting tube has self-heating device, begins automatic heat preservation after heating to 260 ℃, prevents gas condensation such as vapor.
(3) The samples were subjected to TGA-FTIR testing, respectively;
in the step (3), the samples N are respectively mixedSilicone rubberAnd NBase rubberPlacing in a TGA experimental instrument, and recording its weight as MSilicone rubberAnd MBase rubberAnd starting a TGA test, and simultaneously starting an FTIR test when the TGA test device reaches the lowest test temperature and the nitrogen gas is introduced into the device for not less than 30 min.
The 3# silicone rubber sample was placed into the TGA laboratory instrument with clean tweezers to obtain its weight, M3# silicon rubberAnd starting a TGA test, and simultaneously starting an FTIR test when the TGA test device reaches the specified test temperature and is introduced with nitrogen for no less than 30 min. After the test is finished, respectively putting the No. 4 silicone rubber sample and the base rubber sample into a TGA experimental instrument by using clean tweezers, and repeating the test to obtain MNo. 4 silicone rubber，MBase rubber。
(4) The hydrophobic endurance performance is characterized;
selecting a sample NSilicone rubberHas a wave number of 2960 +/-15 cm in FTIR test data-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureHydrophobicityObtaining the area S of the area and the surrounding city of the abscissaHydrophobicityFurther obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialHydrophobicity=SHydrophobicity/MSilicone rubber。
FTIR test data of 3# and 4# silicone rubber materials respectively selected have wave number of 2960 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity Y3# Silicone rubber, 2960、YNo. 4 Silicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperature3# Water repellency、LWater repellency of No. 4Obtaining the area S of the area and the surrounding city of the abscissa3# Water repellency，SWater repellency of No. 4Further obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber material3# Water repellency=S3# Water repellency/ M3# silicon rubber，kWater repellency of No. 4= SWater repellency of No. 4/MNo. 4 silicone rubber。
(5) Calculating the content of the base rubber;
in the step (5), a sample N is selectedSilicone rubberAnd NBase rubberThe wave number in FTIR test data is 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureSilicone rubber、LSilicone rubberObtaining the area S of the area and the surrounding city of the abscissaSilicone rubber、SBase rubberFurther calculating the base rubber content k of the silicon rubber materialBase rubber=SSilicone rubber×MBase rubber/（SBase rubber×MSilicone rubber）。
Selected base and silicon rubber material FTIR test data has the wave number of 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity Y3# Silicone rubber, 3015、YNo. 4 Silicone rubber, 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperature3# silicon rubber、LNo. 4 silicone rubber、LBase rubberObtaining the area S of the area and the surrounding city of the abscissa3# silicon rubber=5.894，SNo. 4 silicone rubber=3.996， SBase rubber=9.452, and calculating the content k of the base rubber of the silicon rubber material3# base rubber=S3# silicon rubber×MBase rubber/（SBase rubber×M3# silicon rubber）；k4# base rubber=SNo. 4 silicone rubber×MBase rubber/（SBase rubber×MNo. 4 silicone rubber）。
(6) And (4) evaluating the quality of the silicon rubber material.
And (4) evaluating the quality of the silicon rubber material. k is a radical of3# Water repellencyAnd k3# base rubberAll values are greater than kWater repellency of No. 4And k4# base rubberAnd the quality of the 3# silicon rubber material is better than that of the 4# silicon rubber material.
Example 3
(1) Preparing samples, namely cutting samples from the cured silicone rubber material and the used base rubber thereof respectively;
selecting two proportions of composite insulators produced by a certain manufacturer, and cutting off a piece of composite insulator at the umbrella skirt part of the composite insulator by using a wallpaper cutter to be used as a test silicon rubber sample NSilicone rubberRespectively recorded as # 5 and # 6. 5# and 6# are silicone rubber materials with different proportions made of the same base rubber and filler. The sample weight was 20. + -.3 mg. Cutting the base rubber used by the silicon rubber material by a wallpaper cutter to be used as a test base rubber sample NBase rubber(ii) a The 5# and 6# samples have similar shapes and structures, the surface of the samples is wiped with absolute ethyl alcohol to be dirty, and the samples are placed in a dust cover and naturally dried.
(2) And the gas measuring unit of the FTIR experimental instrument is connected with the TGA test unit, and test parameters are set.
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;
the TGA test apparatus was opened and the parameters of the TGA laboratory instrument were set:
setting the test atmosphere as nitrogen, the gas flow rate as 70ml/min, the test minimum temperature as 20 ℃, the test maximum temperature as 800 ℃ and the heating rate as 20 ℃/min.
The FTIR test device is opened, and FTIR test parameters are set:
the measurement interval was 3 times/s;
after FTIR laboratory glassware gas measurement unit is connected with TGA test unit, the connecting tube has self-heating device, begins automatic heat preservation after heating to 200 ℃, prevents gas condensation such as vapor.
(3) The samples were subjected to TGA-FTIR testing, respectively;
in the step (3), the samples N are respectively mixedSilicone rubberAnd NBase rubberPlacing in a TGA experimental instrument, and recording its weight as MSilicone rubberAnd MBase rubberAnd starting a TGA test, and simultaneously starting an FTIR test when the TGA test device reaches the lowest test temperature and the nitrogen gas is introduced into the device for not less than 30 min.
The 5# silicone rubber sample was placed into the TGA laboratory instrument with clean tweezers to obtain its weight, M5# silicon rubberAnd starting a TGA test, and simultaneously starting an FTIR test when the TGA test device reaches the specified test temperature and is introduced with nitrogen for no less than 30 min. After the test is finished, respectively putting the 5# silicon rubber sample and the base rubber sample into a TGA experimental instrument by using clean tweezers, and repeating the test to obtain M5# silicon rubber，MBase rubber。
(4) The hydrophobic endurance performance is characterized;
selecting a sample NSilicone rubberHas a wave number of 2960 +/-15 cm in FTIR test data-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureHydrophobicityObtaining the area S of the area and the surrounding city of the abscissaHydrophobicityFurther obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialHydrophobicity=SHydrophobicity/MSilicone rubber。
FTIR test data of 5# and 6# silicon rubber materials respectively selected have wave number of 2960 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YNo. 5 Silicone rubber, 2960、YNo. 6 Silicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureHydrophobicity of 5#、LWater repellency of No. 6Obtaining the area S of the area and the surrounding city of the abscissaHydrophobicity of 5#，SWater repellency of No. 6Further obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialHydrophobicity of 5#=S5# hydrophobicProperty of (2)/ M5# silicon rubber，kWater repellency of No. 6= SWater repellency of No. 6/M6# silicon rubber。
(5) Calculating the content of the base rubber;
in the step (5), a sample N is selectedSilicone rubberAnd NBase rubberThe wave number in FTIR test data is 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureSilicone rubber、LSilicone rubberObtaining the area S of the area and the surrounding city of the abscissaSilicone rubber、SBase rubberFurther calculating the base rubber content k of the silicon rubber materialBase rubber=SSilicone rubber×MBase rubber/（SBase rubber×MSilicone rubber）。
Selected base and silicon rubber material FTIR test data has the wave number of 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity Y5# Silicone rubber, 3015、Y6# Silicone rubber, 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperature5# silicon rubber、L6# silicon rubber、LBase rubberObtaining the area S of the area and the surrounding city of the abscissa5# silicon rubber，S6# silicon rubber， SBase rubberFurther calculating the base rubber content k of the silicon rubber material5# base rubber=S5# silicon rubber×MBase rubber/（SBase rubber×M5# silicon rubber）；k6# base rubber=S6# silicon rubber×MBase rubber/（SBase rubber×M6# silicon rubber）。
(6) And (4) evaluating the quality of the silicon rubber material.
And (4) evaluating the quality of the silicon rubber material. KHydrophobicity of 5#And k5# base rubberAll values are greater than kWater repellency of No. 6And k6# base rubberAnd the quality of the 5# silicon rubber material is better than that of the 6# silicon rubber material.
Example 4
(1) Preparing samples, namely cutting samples from the cured silicone rubber material and the used base rubber thereof respectively;
selecting two proportions of composite insulators produced by a certain manufacturer, and cutting off a piece of composite insulator at the umbrella skirt part of the composite insulator by using a wallpaper cutter to be used as a test silicon rubber sample NSilicone rubberRespectively recorded as 7#, 8 #. No. 7 and No. 8 are silicone rubber materials with different proportions and made of the same base rubber and filler. The sample weight was 20. + -.3 mg. Cutting the base rubber used by the silicon rubber material by a wallpaper cutter to be used as a test base rubber sample NBase rubber(ii) a The 7# and 8# samples have similar shapes and structures, the surface of the samples is wiped with absolute ethyl alcohol to remove dirt, and the samples are placed in a dustproof cover and naturally dried.
(2) The gas measuring unit of the FTIR experimental instrument is connected with the TGA experimental instrument, and experimental parameters are set.
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;
the TGA test apparatus was opened and the parameters of the TGA laboratory instrument were set:
setting the test atmosphere as nitrogen, the gas flow rate as 60ml/min, the test minimum temperature as 24 ℃, the test maximum temperature as 780 ℃ and the heating rate as 29 ℃/min.
The FTIR test device is opened, and FTIR test parameters are set:
the measurement interval was 2 times/s;
after the gas measurement unit of the FTIR experimental instrument is connected with the TGA test unit, an automatic heating device is arranged in a connecting pipeline, and the gas measurement unit starts to automatically preserve heat after being heated to 230 ℃.
(3) The samples were subjected to TGA-FTIR testing, respectively;
in the step (3), the samples N are respectively mixedSilicone rubberAnd NBase rubberPlacing in a TGA experimental instrument, and recording its weight as MSilicone rubberAnd MBase rubberAnd starting a TGA test, and simultaneously starting an FTIR test when the TGA test device reaches the lowest test temperature and is introduced with nitrogen for no less than 30 min.
The 7# silicone rubber sample was placed into the TGA laboratory instrument with clean tweezers to obtain its weight, M7# silicon rubberAnd starting a TGA test, and simultaneously starting an FTIR test when the TGA test device reaches the specified test temperature and is introduced with nitrogen for no less than 30 min. After the test is finished, respectively putting the 7# silicon rubber sample and the base rubber sample into a TGA experimental instrument by using clean tweezers, and repeating the test to obtain M7# silicon rubber，MBase rubber。
(4) The hydrophobic endurance performance is characterized;
selecting a sample NSilicone rubberHas a wave number of 2960 +/-15 cm in FTIR test data-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureHydrophobicityObtaining the area S of the area and the surrounding city of the abscissaHydrophobicityFurther obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialHydrophobicity=SHydrophobicity/MSilicone rubber。
FTIR test data of 7# and 8# silicon rubber materials respectively selected have wave number of 2960 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity Y7# Silicone rubber, 2960、Y8# Silicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureWater repellency of 7 #)、LWater repellency of No. 8Obtaining the area S of the area and the surrounding city of the abscissaWater repellency of 7 #)，SWater repellency of No. 8Further obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialWater repellency of 7 #)=SWater repellency of 7 #)/ M7# silicon rubber，kWater repellency of No. 8= SWater repellency of No. 8/M8# silicon rubber。
(5) Calculating the content of the base rubber;
in the step (5), a sample N is selectedSilicone rubberAnd NBase rubberThe wave number in FTIR test data is 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureSilicone rubber、LSilicone rubberObtaining the area S of the area and the surrounding city of the abscissaSilicone rubber、SBase rubberFurther calculating the base rubber content k of the silicon rubber materialBase rubber=SSilicone rubber×MBase rubber/（SBase rubber×MSilicone rubber）。
Selected base and silicon rubber material FTIR test data has the wave number of 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity Y7# Silicone rubber, 3015、Y8# Silicone rubber, 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperature7# silicon rubber、L8# silicon rubber、LBase rubberObtaining the area S of the area and the surrounding city of the abscissa7# silicon rubber，S8# silicon rubber， SBase rubberFurther calculating the base rubber content k of the silicon rubber material7# base rubber=S7# silicon rubber×MBase rubber/（SBase rubber×M7# silicon rubber）；k8# base rubber=S8# silicon rubber×MBase rubber/（SBase rubber×M8# silicon rubber）。
(6) And (4) evaluating the quality of the silicon rubber material.
And (4) evaluating the quality of the silicon rubber material. KWater repellency of No. 8And k8# base rubberAll values are greater than kWater repellency of 7 #)And k7# base rubberAnd the quality of the 8# silicon rubber material is better than that of the 7# silicon rubber material.
Claims (10)
1. A silicon rubber material quality evaluation method based on TGA-FTIR is characterized in that: which comprises the following steps of,
(1) preparing samples, namely cutting samples from the cured silicone rubber material and the used base rubber thereof respectively;
(2) the gas measurement unit of the FTIR experimental instrument is connected with the test unit of the TGA experimental instrument, and test parameters are set;
(3) the samples were subjected to TGA-FTIR testing, respectively;
(4) the hydrophobic endurance performance is characterized;
(5) calculating the content of the base rubber;
(6) and (4) evaluating the quality of the silicon rubber material.
2. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in step (1), the sample weight was 20. + -.3 mg.
3. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: the samples cut out in the step (1) are respectively NSilicone rubberAnd NBase rubber；
And (2) removing dirt on the surface of the sample by using absolute ethyl alcohol in the step (1), and placing the sample in a dust cover for naturally drying.
4. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in the step (2), after a gas measurement unit of the FTIR experimental instrument is connected with a TGA test unit, the whole device is replaced by nitrogen, the nitrogen is continuously introduced, and then test parameters are set;
parameters for the TGA laboratory instrument were set:
the TGA experimental apparatus is in a test atmosphere of nitrogen, the gas flow rate is not less than 40-70ml/min, the lowest test temperature is set to be 20-30 ℃, the highest test temperature is 750-.
5. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 1, wherein: in step (2), FTIR test parameters are set:
the measurement interval is not less than 1 time/s;
after the FTIR experimental instrument gas measurement unit is connected with the TGA test unit, the connecting pipeline is provided with an automatic heating device, and the temperature is automatically preserved after the gas measurement unit is heated to the temperature not lower than 200 ℃.
6. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 3, wherein: in the step (3), the samples N are respectively mixedSilicone rubberAnd NBase rubberPlaced in a TGA laboratory instrument and recorded as M in weightSilicone rubberAnd MBase rubberAnd respectively starting TGA tests, and simultaneously starting FTIR tests when the TGA test device reaches the set lowest test temperature and the nitrogen gas introduction time of the whole device is not less than 30 min.
7. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 6, wherein: in the step (4), a sample N is selectedSilicone rubberHas a wave number of 2960 +/-15 cm in FTIR test data-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber, 2960Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureHydrophobicityObtaining the area S of the area and the surrounding city of the abscissaHydrophobicityFurther obtaining the hydrophobic endurance property characterization quantity k of the silicon rubber materialHydrophobicity=SHydrophobicity/MSilicone rubber。
8. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 7, wherein: in the step (5), a sample N is selectedSilicone rubberAnd NBase rubberThe wave number in FTIR test data is 3015 +/-15 cm-1The maximum value of the middle absorbance peak is used as the characteristic quantity YSilicone rubber 3015、YBase glue, 3015Drawing the change curve L of the temperature change of the sample with the test time or the test temperatureSilicone rubber、LSilicone rubberObtaining the area S of the area and the surrounding city of the abscissaSilicone rubber、SBase rubberFurther calculating the base rubber content k of the silicon rubber materialBase rubber=SSilicone rubber×MBase rubber/（SBase rubber×MSilicone rubber）。
9. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 8, wherein: in step (6), according to kHydrophobicityAnd kBase rubberThe values were evaluated.
10. The TGA-FTIR-based silicone rubber material quality assessment method according to claim 9, wherein: k is a radical ofHydrophobicityAnd kBase rubberThe larger the value, the better the quality of the silicone rubber material; conversely, the poorer the quality of the silicone rubber material.
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