CN109521041B - XLPE material thermal aging dynamic process multiphase combined detection method - Google Patents
XLPE material thermal aging dynamic process multiphase combined detection method Download PDFInfo
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- 229920003020 cross-linked polyethylene Polymers 0.000 title claims abstract description 83
- 239000004703 cross-linked polyethylene Substances 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000008569 process Effects 0.000 title claims abstract description 18
- 238000003878 thermal aging Methods 0.000 title claims abstract description 17
- 238000001514 detection method Methods 0.000 title claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 86
- 230000008859 change Effects 0.000 claims abstract description 50
- 238000002844 melting Methods 0.000 claims abstract description 25
- 230000008018 melting Effects 0.000 claims abstract description 25
- 238000004458 analytical method Methods 0.000 claims abstract description 24
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 230000007246 mechanism Effects 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 7
- 238000004817 gas chromatography Methods 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims abstract description 3
- 230000008025 crystallization Effects 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 25
- 239000013078 crystal Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000003595 spectral effect Effects 0.000 claims description 7
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 5
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 claims description 5
- 238000005102 attenuated total reflection Methods 0.000 claims description 4
- 238000000113 differential scanning calorimetry Methods 0.000 claims description 4
- 125000000524 functional group Chemical group 0.000 claims description 4
- 238000002441 X-ray diffraction Methods 0.000 claims description 3
- 238000012844 infrared spectroscopy analysis Methods 0.000 claims description 3
- 238000010606 normalization Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000012935 Averaging Methods 0.000 claims description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 2
- 238000002835 absorbance Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 230000002596 correlated effect Effects 0.000 claims 1
- 230000008030 elimination Effects 0.000 claims 1
- 238000003379 elimination reaction Methods 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 7
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 239000007790 solid phase Substances 0.000 abstract description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 5
- 238000009413 insulation Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000001307 laser spectroscopy Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
Abstract
The invention discloses a multiphase combined detection method for a thermal aging dynamic process of an XLPE material, which comprises the following steps: s1, preparing an aged XLPE test piece and gas; s2, cooling to room temperature, and performing Fourier infrared spectrum analysis on the XLPE sample to obtain a Fourier infrared spectrum curve; s3, drawing C, O and a change curve of the strength of the H element along with the aging time; s4, determining the type of the gas released in the aging process through gas chromatography analysis to obtain a change curve of the gas content along with the aging time; s5, determining the change curve of the crystalline region content in the material at each aging stage; s6, determining the enthalpy of melting of material crystallization and the change curve of melting initial temperature along with aging time; and S7, presuming the aging mechanism of the XLPE material according to the obtained change curve. The method comprises gas phase analysis, solid phase analysis and crystalline phase analysis of the aging process, and can comprehensively reflect the material decomposition mechanism of the aging process of XLPE.
Description
Technical Field
The invention relates to monitoring of an aging state and a dynamic aging development process of XLPE (cross linked polyethylene), in particular to a multiphase combined detection method for a thermal aging dynamic process of an XLPE material.
Background
The cross-linked polyethylene (XLPE) material has good heat resistance, electrical properties, and mechanical strength, and is widely used in the insulation part of the ultra-high voltage power cable. With the increase of the complexity of the cable laying environment in China, the dynamic monitoring of the aging process of the XLPE insulating material under complex conditions becomes more important.
Aging of the cable insulation after long-term operation is one of the main causes of XLPE cable damage. The thermal aging process of the XLPE cable insulation material is that the chemical bond is broken due to the action of heat on material molecules, so that the molecular weight and the crosslinking degree of the XLPE material are reduced, and the aging and even insulation failure of the XLPE material are caused. At present, the description of the aging dynamic process of the XLPE is the change rule of the performance of the XLPE material along with the aging time, and the aging process is analyzed from the aspects of element change and decomposition substances of the material. Therefore, the XLPE material thermal aging dynamic process multiphase combined detection method can provide a new idea for aging mechanism analysis of XLPE.
Disclosure of Invention
The invention provides a multiphase combined detection method for an XLPE material thermal aging dynamic process in order to overcome the defects of the prior art. The method comprises gas phase analysis, solid phase analysis and crystalline phase analysis of the aging process, and can comprehensively reflect the material decomposition mechanism of the aging process of XLPE.
The invention is realized by the following technical scheme:
a heterogeneous joint detection method for an XLPE material thermal aging dynamic process comprises the following steps:
s1, preparing XLPE test pieces according to a common formula of a cable, aging the XLPE test pieces in a closed small aging box at the temperature of 160-200 ℃ for a set time, taking out a group of XLPE test pieces and a bag of gas at regular intervals, wherein each group of XLPE test pieces comprises a plurality of XLPE test pieces;
s2, cooling to room temperature, carrying out Fourier infrared spectrum analysis on the XLPE sample after 24 hours to obtain a Fourier infrared spectrum curve reflecting the change of organic functional groups in the material and the oxidation degree;
s3, extracting the characteristic spectrum peak intensity of C element, O element and H element by LIBS analysis of the XLPE sample, and drawing the variation curve of different element intensities along with aging time;
s4, determining the type of gas released in the aging process by performing gas chromatography on the gas collected at regular intervals to obtain a variation curve of the gas content along with the aging time;
s5, carrying out XRD analysis on the XLPE aging sample, and determining the change curve of the crystalline region content in the material at each aging stage;
s6, carrying out DSC analysis on the XLPE aged sample, and determining the crystal melting enthalpy of the material and the change curve of the melting initial temperature along with the aging time;
s7, carrying out normalization processing on the curves obtained in the steps S2, S3, S4, S5 and S6 to obtain the change rule of each parameter along with the aging time, and accordingly, the aging mechanism of the XLPE material is estimated.
Further, in step S1, the aging time is 0h, 6h, 12h, 18h, 24h and 30h, and a set of XLPE samples and a bag of gas are taken out every 6h, wherein each set of XLPE samples comprises 3 XLPE test pieces.
Further, the length, width and thickness of the XLPE test piece were 30mm 10mm 1mm, respectively.
Further, in step S2, the change of the organic functional group in the material was obtained by specifically calculating 1720cm of carbonyl band associated with oxidative aging characteristics-1With a band 2010cm which is not altered by thermo-curing aging-1The ratio of absorbance of (a).
Further, in step S2, infrared spectroscopic analysis of XLPE sample is performed by physical and chemical analysis of the sample with IRaffinity-1S Fourier transform infrared spectrometer of Shimadzu corporation, and the measurement is performed in attenuated total reflection mode with 20 scanning times and 2cm resolution-1The scanning range is 500-4000 cm-1。
Further, in step S3, the plotting of the intensity of different elements as a function of aging time includes the steps of excluding the significant error points and averaging the spectral intensities of the remaining points.
Further, in step S4, before the change of the gas content with the aging time is plotted, the ratio of different gases to the total gas content is calculated, and then a change curve of the ratio with the aging time is plotted.
Further, in step S5, when determining the change of the content of the crystalline region in the material at each aging stage, the XRD curve is subjected to Guass peak-splitting fitting, the ratio of two sharp peak areas to the total area of the spectral line is calculated to obtain the crystallinity, and finally, a change curve of the crystallinity along with the aging time is drawn.
Further, when determining the enthalpy of melting of the material crystal and the change rule of the melting start temperature along with the aging time in step S6, the method first performs the operation of removing the thermal history on the material, and specifically includes: firstly heating to the maximum temperature for a certain time, then cooling to room temperature at the same speed for a certain time, then obtaining a melting curve, melting enthalpy and melting temperature again at the previous heating speed, and finally respectively drawing the change curves of the melting enthalpy and the melting temperature along with the aging time.
Further, in step S6, the material is heated to 150 ℃, kept at a constant temperature for 5min, then cooled to room temperature at a rate of 10 ℃/min, and finally heated at a rate of 10 ℃/min to obtain a melting curve.
Compared with the prior art, the multi-phase joint detection method for the thermal ageing dynamic process of the XLPE material, provided by the invention, comprises gas-phase analysis, solid-phase analysis and crystalline-phase analysis of the ageing process, can comprehensively reflect the material decomposition mechanism of the XLPE ageing process, and provides a new idea for the ageing mechanism analysis of the XLPE.
Drawings
FIG. 1 is a flow chart of the dynamic process polyphase joint detection method of the present invention.
FIG. 2 is a Fourier infrared spectrum of an XLPE sample of the present invention as a function of aging time.
FIG. 3 is a graph showing the change of the content of element C in the sample according to the present invention with aging time.
FIG. 4 is a graph showing the change of the O element content of the sample according to the present invention with aging time.
FIG. 5 is a graph showing the change of the H element content of the sample according to the present invention with aging time.
FIG. 6 is a graph showing the change in the isobutylene content of the samples of the present invention with respect to the heat aging time.
FIG. 7 is a graph showing the change in the crystalline region content of the sample according to the present invention.
FIG. 8 is graphs showing the enthalpy of crystal fusion and the melting initiation temperature of the sample according to the present invention as a function of aging time.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
As shown in fig. 1, a method for detecting heterogeneous combination of thermal aging dynamic process of XLPE material includes the following steps:
s1, preparing XLPE test pieces according to a common formula of a cable, aging at 160-200 ℃ for accelerating a thermal aging process, wherein the aging time is 0h, 6h, 12h, 18h, 24h and 30h, taking out a group of XLPE test pieces and a bag of gas every 6h, and each group of XLPE test pieces comprises 3 XLPE test pieces; keeping the size of the sample the same, wherein the length, the width and the thickness of the XLPE sample are respectively 30mm multiplied by 1 mm;
s2, after cooling to room temperature for 24 hours, carrying out Fourier infrared spectrum analysis on the XLPE sample under each thermal aging time, and detecting to obtain a change curve of a chemical group at a position of 1-10 mu m on the surface of the XLPE material; in order to describe the dynamic change process of the aging degree, the appearance and the enhancement of carbonyl peak under different thermal aging time are mainly used as one of the measures of the aging degree, as shown in FIG. 2;
s3, LIBS analysis is carried out on the XLPE sample, the same position on the surface of the XLPE sample is bombarded by multiple times of pulse laser, an element spectrogram of the XLPE sample under different thermal ageing times after the first 30 times of bombardment is obtained, an entropy weight method is adopted to carry out mean value analysis on the 30 element spectrograms, the characteristic spectral peak intensities of C elements, O elements and H elements under different thermal ageing times are extracted, a change curve of the characteristic peak intensities of different elements along with the thermal ageing time is drawn, as shown in FIG. 3, when a change curve graph of the different element intensities along with the ageing time is drawn, obvious error points are eliminated, and then the spectral intensities of the rest points are averaged;
s4, performing gas chromatography analysis on gases generated by an XLPE sample at different thermal ageing stages, analyzing and comparing characteristic peaks in a chromatogram in order to determine organic gases possibly represented by the peaks, finally extracting the highest peak of the gas chromatogram, namely isobutene, in combination with a cross-linked structure of cross-linked polyethylene, analyzing, and drawing isobutene content change curves at different thermal ageing times, wherein as shown in FIG. 6, before drawing the change of the gas content along with the ageing time, the ratio of different gases to the total gas content is calculated, and then the change curve of the ratio along with the ageing time is drawn;
s5, carrying out XRD analysis on XLPE samples under different thermal ageing times, calculating the ratio of different crystal face diffraction peak areas of crystals in the XLPE material through Gauss peak-splitting fitting in order to quantitatively analyze the change of the crystallinity of the XLPE material, and obtaining the change rule of the XLPE material crystals along with the ageing time, wherein a specific change curve is shown in figure 7;
s6, carrying out DSC analysis on XLPE under different thermal ageing times, heating the material to 150 ℃, keeping the temperature constant for 5min to eliminate thermal history, cooling and crystallizing at the speed of 10 ℃/min to room temperature, heating to 150 ℃ again to obtain the melting peak area of the XLPE material, representing the change of energy required by melting the XLPE material crystal, and revealing the change rule of the crystal region in the XLPE material from the other side, as shown in FIG. 8;
s7, carrying out normalization processing on the curves obtained in the steps S2, S3, S4, S5 and S6 to obtain the change rule of each parameter along with the aging time, and accordingly, the aging mechanism of the XLPE material is estimated.
In this example, the trend of the change of the carbonyl content of the sample can be visually reflected by performing fourier infrared spectroscopy analysis on the sample, and as shown in fig. 2, the carbonyl content increases with the increase of the thermal aging time.
Fig. 3 to 5 are the content change curves of the C, O, H element of the sample at aging times of 0h, 6h, 12h, 18h, 24h and 30h, respectively, and it can be seen from the curves that the change slope of the C, O element content suddenly increases at 12 to 18h and the content of C, O, H element increases with the increase of the thermal aging time.
In this example, the Fourier Infrared spectrometer was analyzed by IRaffinity-1S from Shimadzu corporation, Japan, as Attenuated Total reflection (Attenuated Total reflection)Station, ATR) mode measurement, scanning times of 20 times, resolution of 2cm-1The scanning range is 500-4000 cm-1。
Laser Induced Breakdown Spectroscopy (LIBS) a J200 laser spectroscopy elemental analyzer, a LIBS device from american application spectroscopy corporation, was used.
The gas chromatography is analyzed by adopting a gas mass spectrometer HP5973GCMS of Hewlett-packard company in America, the mass range is 1.5-800u, and the scanning speed is 5000-10000 u/sec.
The X-ray polycrystalline diffraction adopts an X-ray diffractometer D8 model of Bruker company in Germany to carry out XRD crystallization area content analysis, and the angle measurement accuracy reaches up to 0.01 degrees.
Differential scanning calorimetry DSC214 type differential scanning calorimeter of German Nachi company is adopted to carry out DSC experiment on XLPE samples, each sample is about 5mg, the atmosphere is nitrogen, the heating rate is 10K/min, and the temperature range is 30-140 ℃.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention and are intended to be equivalent substitutions are included in the scope of the present invention.
Claims (3)
1. A heterogeneous joint detection method for an XLPE material thermal aging dynamic process is characterized by comprising the following steps:
s1, preparing XLPE test pieces according to a common formula of a cable, aging in a closed small aging box at the temperature of 160-200 ℃ for a set time, taking out a group of XLPE test pieces and a pack of gas at regular intervals, wherein each group of XLPE test pieces comprises a plurality of XLPE test pieces; aging for 0h, 6h, 12h, 18h, 24h and 30h respectively, taking out a group of XLPE samples and a pack of gas every 6h, wherein each group of XLPE samples comprises 3 XLPE test pieces; the length, width and thickness of the XLPE test piece are respectively 30mm x 10mm x 1 mm;
s2, cooling to room temperature, carrying out Fourier infrared spectrum analysis on the XLPE sample after 24h to obtain Fourier reflecting the change of organic functional groups in the material and the oxidation degreeLeaf infrared spectral curve; the change in the organic functional groups in the material was obtained by calculating, in particular, the carbonyl band 1720cm which is correlated with the oxidative ageing characteristics-1With a band 2010cm which is not altered by thermal oxygen aging-1The ratio of absorbance of (a); performing infrared spectroscopic analysis on XLPE sample, performing physicochemical analysis on the sample by using IRaffinity-1S type Fourier transform infrared spectrometer of Shimadzu corporation, measuring according to attenuated total reflection mode, scanning for 20 times, and resolution of 2cm-1The scanning range is 500-4000 cm-1;
S3, extracting the characteristic spectrum peak intensity of C element, O element and H element by LIBS analysis of the XLPE sample, and drawing the variation curve of different element intensities along with aging time;
s4, determining the type of gas released in the aging process by performing gas chromatography on the gas collected at regular intervals to obtain a variation curve of the gas content along with the aging time;
s5, carrying out XRD analysis on the XLPE aging sample, and determining the change curve of the crystalline region content in the material at each aging stage; when the change of the content of the crystalline region in the material at each aging stage is determined, firstly carrying out Guass peak-splitting fitting on an XRD curve, calculating the ratio of two sharp peak areas to the total area of a spectral line to obtain the crystallinity, and finally drawing a change curve of the crystallinity along with the aging time;
s6, carrying out DSC analysis on the XLPE aged sample, and determining the crystal melting enthalpy of the material and the change curve of the melting initial temperature along with the aging time; when determining the enthalpy of crystallization and melting of the material and the change rule of the melting initial temperature along with the aging time, firstly, the thermal history elimination operation is carried out on the material, and the method specifically comprises the following steps: firstly heating to the highest temperature for a certain time, then cooling to room temperature at the same speed for a certain time, then obtaining a melting curve, melting enthalpy and melting temperature again at the previous heating speed, and finally respectively drawing a change curve of the melting enthalpy and the melting temperature along with aging time; heating the material to 150 ℃, keeping the constant temperature for 5min, then cooling to room temperature at a speed of 10 ℃/min, and finally heating at a speed of 10 ℃/min to obtain a melting curve;
s7, carrying out normalization processing on the curves obtained in the steps S2, S3, S4, S5 and S6 to obtain the change rule of each parameter along with the aging time, and accordingly, the aging mechanism of the XLPE material is estimated.
2. The method for multiphase joint detection of the XLPE material thermal aging dynamic process as claimed in claim 1, wherein the step of plotting the intensity of different elements as a function of aging time in step S3 comprises the steps of excluding the significant error points and averaging the spectral intensities of the remaining points.
3. The method for multi-phase combined detection of the dynamic process of thermal aging of XLPE material as claimed in claim 1, wherein in step S4, before plotting the change of gas content with aging time, the ratio of different gases to the total gas content is calculated, and then the change curve of the ratio with aging time is plotted.
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CN113552109B (en) * | 2020-04-23 | 2023-12-29 | 中国石油化工股份有限公司 | Memory, and method, device and equipment for testing and analyzing reaction thermal effect based on Raman spectrum |
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CN111721624B (en) * | 2020-06-03 | 2023-06-16 | 中广核三角洲(太仓)检测技术有限公司 | Nuclear PEEK material thermal aging mechanism evaluation method based on crystallinity |
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