CN107817258B - Liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak-splitting fitting - Google Patents
Liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak-splitting fitting Download PDFInfo
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Abstract
A liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak-splitting fitting comprises the following specific steps: 1S samples from the liquid silicone rubber to be tested. 2S, carrying out X-ray diffraction analysis on the sample, carrying out peak-splitting fitting on the X-ray diffraction maps of the inner layer and the surface layer, calculating the ratio of the integral areas of corresponding diffraction peaks of PDMS and white carbon black, and comparing the ratio of the surface layer and the inner layer so as to judge the aging degree of the liquid silicone rubber; the ratio of the integral areas of the corresponding diffraction peaks of the white carbon black and the PDMS is marked as XSiO 2/PDMS; and 3S, the aging degree of the sample is judged, and the method has the advantages of providing more accurate aging degree evaluation of the liquid silicone rubber material of the power station equipment, perfecting the aging evaluation procedure of the equipment and laying a foundation for a reliable maintenance strategy formulated by a transportation and inspection department.
Description
Technical Field
The invention relates to the technical field of material performance evaluation, in particular to a liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak-splitting fitting.
Background
The silicon rubber is a composite insulating material commonly used in power systems, is widely applied in the field of high-voltage external insulation, is a higher-grade silicon rubber developed in the 70 s, and is characterized in that: the crosslinking is completed by the addition reaction of vinyl siloxane and hydrosilyl; the molecular weight is small, the viscosity of the rubber material is low, and the rubber material is easy to process and form; the vulcanization can be carried out at room temperature or accelerated by increasing the temperature. Compared with the condensed silicone rubber, the silicone rubber has the characteristics of deep vulcanization, no by-product, small shrinkage rate and the like.
The liquid silicon rubber is widely used in 110 kV-500 kV substations of national power grids and southern power grids as an outer insulating sheath of a mutual inductor. In recent years, the liquid silicon rubber outer insulation sheath used in southern power grid part areas has serious aging phenomena such as hydrophobicity reduction, cracking, pulverization and the like, and the normal operation of equipment is greatly influenced. Therefore, the aging state of the liquid silicone rubber is accurately evaluated by detecting various performance parameters of the liquid silicone rubber, and the method has important guiding significance and engineering value for operation and maintenance work of power station equipment.
X-ray diffraction analysis is a method of analyzing the crystal structure, parameters, and defects of a material using the diffraction phenomenon of X-rays in a crystal. The main component of the liquid silicone rubber is Polydimethylsiloxane (PDMS), and the liquid silicone rubber contains more white carbon black filler. Because of its excellent properties, liquid silicone rubbers generally do not require the addition of aluminum hydroxide fillers to improve tracking resistance. The composition of the silica filler is similar to the siloxane backbone, and it is difficult to completely distinguish between the two in elemental and functional group analysis. However, in an XRD diffraction pattern, the peak positions of the white carbon black filler and the siloxane are different and can be distinguished through peak separation fitting.
In the aged liquid silicone rubber, the side chain organic groups of PDMS are oxidized and crosslinked to increase, which is reflected by the obvious decrease of the content of organic components and the increase of the content of inorganic components (including white carbon black filler and SiO 2-like structure in the PDMS crosslinked structure). The integral intensity of the diffraction peak of XRD is in direct proportion to the content of the corresponding phase, so that the integral intensity of the diffraction peak of PDMS and white carbon black can be calculated through peak-splitting fitting, the components of the liquid silicone rubber material can be quantitatively analyzed, and the aging degree of the material can be more accurately evaluated by a maintenance department, so that a corresponding operation maintenance strategy can be formulated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak fitting for judging the component change of the liquid silicone rubber surface layer by analyzing the X-ray diffraction spectrums of the surface layer and the inner layer of the liquid silicone rubber, wherein the test method is suitable for the detection test and the aging degree evaluation of a liquid silicone rubber material without aluminum hydroxide filler.
The invention is realized by the following technical scheme:
a liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak-splitting fitting comprises the following specific steps:
1S samples from the liquid silicone rubber to be tested.
2S, carrying out X-ray diffraction analysis on the sample, carrying out peak-splitting fitting on the X-ray diffraction maps of the inner layer and the surface layer, calculating the ratio of the integral areas of corresponding diffraction peaks of PDMS and white carbon black, and comparing the ratio of the surface layer and the inner layer so as to judge the aging degree of the liquid silicone rubber; the ratio of the integral areas of the corresponding diffraction peaks of white carbon black and PDMS is marked as XSiO2/PDMS：
Wherein a (SiO2) is an integrated area of a peak corresponding to the white carbon black after the peak separation, a central abscissa of the peak is located at 22 ± 0.1 °, a (PDMS) is an integrated area of a peak corresponding to the PDMS after the peak separation, and a central abscissa of the peak is located at 2 θ ═ 12 ± 0.1 °.
3S, judging the aging degree of the sample, namely the surface layer and the inner layer X of the sampleSiO2/PDMSRatio X ofOuter/inner＝XSiO2/PDMS outer layer/XSiO2/PDMS insideWhen X is presentOuter/innerWhen the temperature is higher than 1.5, judging that the sample is seriously aged and needing to take repairing or replacing measures; when 1.5 > XOuter/innerWhen the temperature is higher than 1, judging that the sample is slightly aged, and further evaluating by combining other detection means; when X is presentOuter/innerWhen the silicone rubber is aged 1, it is judged that the liquid silicone rubber is not aged.
As an improvement of the above scheme, the sampling from the liquid silicone rubber to be detected in step 1 is performed by sampling from the liquid silicone rubber sheath to be detected by using a scalpel, cleaning stains attached to the surface of the sample by using a non-woven fabric dipped with absolute ethyl alcohol, and cutting sample pieces with the length of about 1cm × 1cm and the thickness of 1 to 2mm from the surface layer and the inner layer of the sample after the absolute ethyl alcohol is volatilized, so as to perform X-ray diffraction analysis.
As an improvement of the above scheme, the X-ray diffraction pattern in step 2 is preprocessed before the peak-splitting fitting, and the specific steps are as follows:
2.1S reading an X-ray diffraction pattern, wherein an amorphous dispersion peak appears at a diffraction angle 2 theta of 12 +/-0.1 degrees in the pattern of PDMS, and an amorphous dispersion peak appears at a diffraction angle 2 theta of 22 +/-0.1 degrees in the pattern of white carbon black.
And 2.2S, adjusting the base line of the spectrum to ensure that the whole bottom of the spectrum is smoothly and completely coincided with the base line, and deducting the part below the base line to obtain more accurate diffraction peak data.
And 2.3S, performing peak separation fitting on the diffraction peak data.
The invention has the following beneficial effects: the invention relates to a novel method for evaluating the aging degree of liquid silicone rubber based on the peak fitting of an X-ray diffraction spectrum, which can be combined with the existing evaluation means to provide more accurate evaluation on the aging degree of the liquid silicone rubber material of power station equipment and perfect the aging evaluation program of the equipment, thereby laying a foundation for a reliable maintenance strategy made by a transportation and inspection department.
Drawings
FIG. 1 is an X-ray diffraction pattern of the surface layer of a liquid silicone rubber surface sample sheet in the example.
FIG. 2 is an X-ray diffraction pattern of the inner layer of the liquid silicone rubber skin sample in the examples.
Detailed Description
Examples
A liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak-splitting fitting comprises the following specific steps:
1S, sampling from liquid silicone rubber to be detected; sampling from a liquid silicon rubber sheath to be detected through a scalpel, cleaning dirt attached to the surface of a sample by using a non-woven fabric dipped with absolute ethyl alcohol, and cutting sample pieces with the length and width of about 1cm X1 cm and the thickness of 1-2 mm from the surface layer and the inner layer of the sample after the absolute ethyl alcohol is volatilized so as to perform X-ray diffraction analysis.
2S as shown in fig. 1 and fig. 2, an X-ray diffraction pattern is read, an amorphous dispersion peak appears at a diffraction angle 2 θ of 12 ± 0.1 ° in the pattern of PDMS, and an amorphous dispersion peak appears at a diffraction angle 2 θ of 22 ± 0.1 ° in the pattern of white carbon black.
And 3S, adjusting the base line of the spectrum to ensure that the whole bottom of the spectrum is smoothly and completely coincided with the base line, and deducting the part below the base line to obtain more accurate diffraction peak data.
4S, performing peak-splitting fitting on the X-ray diffraction spectrums of the inner layer and the surface layer, and calculating the PDMS and white carbon black pair
Comparing the ratio of the integral areas of the diffraction peaks and the surface layer and the inner layer so as to judge the aging degree of the liquid silicone rubber; the ratio of the integral areas of the corresponding diffraction peaks of white carbon black and PDMS is marked as XSiO2/PDMS：
Wherein a (SiO2) is an integrated area of a peak corresponding to the white carbon black after the peak separation, a central abscissa of the peak is located at 22 ± 0.1 °, a (PDMS) is an integrated area of a peak corresponding to the PDMS after the peak separation, and a central abscissa of the peak is located at 2 θ ═ 12 ± 0.1 °.
5S, judging the aging degree of the sample, namely the surface layer and the inner layer X of the sampleSiO2/PDMSRatio X ofOuter/inner＝XSiO2/PDMS outer layer/XSiO2/PDMS insideWhen X is presentOuter/innerWhen the temperature is higher than 1.5, judging that the sample is seriously aged and needing to take repairing or replacing measures; when 1.5 > XOuter/innerWhen the temperature is higher than 1, judging that the sample is slightly aged, and further evaluating by combining other detection means; when X is presentOuter/innerThe results obtained for the samples examined according to fig. 1 and 2, with no degradation of the liquid silicone rubber determined as 1, are given in table 1 below:
Xouter/innerAnd (4) judging that the sample is seriously aged if the sample is 1.840 & gt 1.5, and taking repair or replacement measures.
The above detailed description is specific to possible embodiments of the present invention, and the embodiments are not intended to limit the scope of the present invention, and all equivalent implementations or modifications that do not depart from the scope of the present invention are intended to be included within the scope of the present invention.
Claims (2)
1. A liquid silicone rubber aging degree evaluation method based on X-ray diffraction spectrum peak-splitting fitting is characterized by comprising the following specific steps:
1S, sampling from liquid silicone rubber to be detected;
2S, carrying out X-ray diffraction analysis on the sample, carrying out peak-splitting fitting on the X-ray diffraction maps of the inner layer and the surface layer, calculating the ratio of the integral areas of corresponding diffraction peaks of PDMS and white carbon black, and comparing the ratio of the surface layer and the inner layer so as to judge the aging degree of the liquid silicone rubber; the ratio of the integral areas of the corresponding diffraction peaks of white carbon black and PDMS is marked as XSiO2/PDMS：
Wherein, a (SiO2) is the integrated area of the peak corresponding to the white carbon black after peak separation, the central abscissa of the peak is located at 22 ± 0.1 ° 2 θ, a (PDMS) is the integrated area of the peak corresponding to PDMS after peak separation, the central abscissa of the peak is located at 12 ± 0.1 ° 2 θ, an X-ray diffraction pattern is read, an amorphous dispersion peak appears at a diffraction angle of 12 ± 0.1 ° 2 θ of PDMS in the pattern, an amorphous dispersion peak appears at a diffraction angle of 22 ± 0.1 ° 2 θ of white carbon black in the pattern, the pattern base line is adjusted to enable the whole bottom of the pattern to be smoothly and completely coincided with the base line, a part below the base line is deducted to obtain accurate diffraction peak data, and the diffraction peak data is subjected to peak separation fitting;
3S, judging the aging degree of the sample, namely the surface layer and the inner layer X of the sampleSiO2/PDMSRatio X ofOuter/inner＝XSiO2/PDMS outer layer/XSiO2/PDMS insideWhen X is presentOuter/innerWhen the temperature is higher than 1.5, judging that the sample is seriously aged and needing to take repairing or replacing measures; when 1.5 > XOuter/innerWhen the temperature is higher than 1, judging that the sample is slightly aged, and further evaluating by combining other detection means; when X is presentOuter/innerWhen the silicone rubber is aged 1, it is judged that the liquid silicone rubber is not aged.
2. The method for evaluating the aging degree of the liquid silicone rubber based on the peak fitting of the X-ray diffraction pattern according to claim 1, wherein the step 1 is to sample the liquid silicone rubber to be detected, after sampling the liquid silicone rubber to be detected from the liquid silicone rubber sheath by a scalpel, the non-woven fabric dipped with absolute ethyl alcohol is used for cleaning dirt attached to the surface of the sample, and after the absolute ethyl alcohol is volatilized, sample pieces with the length of about 1cm X1 cm and the thickness of 1 to 2mm are cut from the surface layer and the inner layer of the sample to perform X-ray diffraction analysis.
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