CN109521041A - A kind of XLPE material heat ageing dynamic process multiphase associated detecting method - Google Patents
A kind of XLPE material heat ageing dynamic process multiphase associated detecting method Download PDFInfo
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- CN109521041A CN109521041A CN201811455748.5A CN201811455748A CN109521041A CN 109521041 A CN109521041 A CN 109521041A CN 201811455748 A CN201811455748 A CN 201811455748A CN 109521041 A CN109521041 A CN 109521041A
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- 230000032683 aging Effects 0.000 title claims abstract description 90
- 229920003020 cross-linked polyethylene Polymers 0.000 title claims abstract description 89
- 239000004703 cross-linked polyethylene Substances 0.000 title claims abstract description 89
- 239000000463 material Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000004458 analytical method Methods 0.000 claims abstract description 25
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 11
- 238000001157 Fourier transform infrared spectrum Methods 0.000 claims abstract description 9
- 230000000977 initiatory effect Effects 0.000 claims abstract description 6
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 4
- 238000001228 spectrum Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 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
- 230000003595 spectral effect Effects 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000012935 Averaging Methods 0.000 claims description 3
- 238000002441 X-ray diffraction Methods 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 3
- 238000013507 mapping Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000002835 absorbance Methods 0.000 claims description 2
- 230000006866 deterioration Effects 0.000 claims description 2
- 238000002329 infrared spectrum Methods 0.000 claims description 2
- 230000009466 transformation Effects 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 6
- 238000002764 solid phase assay Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 19
- 238000003878 thermal aging Methods 0.000 description 10
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000005102 attenuated total reflection Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 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
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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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
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Abstract
The invention discloses a kind of XLPE material heat ageing dynamic process multiphase associated detecting methods, comprising steps of S1, the XLPE test piece for producing aging and gas；S2, XLPE sample progress FTIR spectrum is analyzed to obtain FTIR spectrum curve after being cooled to room temperature；S3, C, O and H element element-intensities are drawn with the change curve of ageing time；S4, the gaseous species that the release of its ageing process is determined by gas chromatographic analysis, obtain gas content with the change curve of ageing time；S5, the change curve for determining crystal region content in each ageing step material；S6, determine material crystalline melting enthalpy and melt initiation temperature degree with the change curve of ageing time；S7, the agine mechaism that XLPE material is speculated according to gained change curve.The present invention includes the gas phase analysis, solid phase assays and crystal phase analysis of ageing process, can comprehensively reflect the material decomposition mechanism of XLPE ageing process.
Description
Technical field
The present invention relates to the monitoring of XLPE ageing state and aging development trend process, specially a kind of XLPE material heat is old
Change dynamic process multiphase associated detecting method.
Background technique
Crosslinked polyethylene (XLPE) material is due to being answered extensively with good heat resistance, electric property, mechanical strength
Used in EHV XLPE power cable insulated part.With the increase of China's cable laying environment complexity, complex condition XLPE
The dynamic monitoring of insulating materials ageing process becomes particularly important.
The aging of cable insulation material is one of the main reason for causing XLPE cable to damage after longtime running.XLPE cable
The Heat Ageing of insulating materials is the fracture that heat leads to chemical bond to the effect of material molecule, leads to the molecule of XLPE material
Amount and the degree of cross linking reduce, to cause aging or even the failure of insulation of XLPE.At present to the description of XLPE aging dynamic process
All it is changing rule of the XLPE material property with ageing time, rarely has and enter in terms of the element variation of material and decomposed substance
Hand analyzes ageing process.Therefore, XLPE material heat ageing dynamic process multiphase associated detecting method can be the ageing machine of XLPE
Reason analysis provides new approaches.
Summary of the invention
The present invention proposes a kind of XLPE material heat ageing dynamic process to overcome shortcoming and deficiency of the existing technology
Multiphase associated detecting method.This method includes the gas phase analysis, solid phase assays and crystal phase analysis of ageing process, can be comprehensive
Reflect the material decomposition mechanism of XLPE ageing process.
The present invention is achieved through the following technical solutions:
A kind of XLPE material heat ageing dynamic process multiphase associated detecting method, includes the following steps:
S1, XLPE test piece is produced according to cable common prescription, is pressed in the small-sized ageing oven of 160~200 DEG C of closing of temperature range
Setting time carries out aging, takes out one group of XLPE sample and a packet gas at regular intervals, if every group of XLPE sample includes
Dry plate XLPE test piece；
S2, it is cooled to room temperature, FTIR spectrum analysis is carried out to XLPE sample afterwards for 24 hours, obtain organic official in reflection material
It can the variation of group and the FTIR spectrum curve of degree of oxidation；
S3, by carrying out LIBS analysis to XLPE sample, extract the characteristic frequency spectrum peak intensity of C element, O element and H element, draw
Different element-intensities are made with the change curve of ageing time；
S4, by carrying out gas chromatographic analysis to the gas collected at regular intervals, determine the gas of its ageing process release
Type obtains gas content with the change curve of ageing time；
S5, XRD analysis is carried out to XLPE aged samples, determines the change curve of crystal region content in each ageing step material；
S6, dsc analysis is carried out to XLPE aged samples, determines material crystalline melting enthalpy and melt initiation temperature degree with ageing time
Change curve；
S7, it is normalized to obtaining curve in described step S2, S3, S4, S5, S6, obtains each parameter with ageing time
Changing rule, to speculate the agine mechaism of XLPE material.
Further, in step S1, ageing time is respectively 0h, 6h, 12h, 18h, for 24 hours and 30h, takes out one every 6h
Group XLPE sample and a packet gas, every group of XLPE sample include 3 XLPE test pieces.
Further, it is respectively 30mm*10mm*1mm that the length of the XLPE test piece is generous.
It further, is specifically to calculate and deterioration by oxidation spy in step S2, when obtaining the variation of organo-functional group in material
Levy related carbonyl bands of a spectrum 1720cm-1With the bands of a spectrum 2010cm that will not change because of hot endowmentization-1Absorbance ratio.
Further, infrared spectrum analysis is carried out using Japanese Shimadzu Corporation to XLPE sample in step S2
IRAffinity-1S type Fourier Transform Infrared Spectrometer to sample carry out physico-chemical analysis, by decaying be all-trans emission mode measurement, sweep
Retouching number is 20 times, resolution ratio 2cm-1, scanning range is 500~4000cm-1。
Further, in step S3, when shown change curve for drawing different element-intensities with ageing time includes row
The step of spectral intensity of left point is averaging again except obvious errors point.
Further, in step S4, before mapping to gas content with the variation of ageing time, it is total first to calculate gas with various Zhan
The ratio of gas content, then ratio is drawn with the change curve of ageing time.
Further, in step S5, when determining the variation of crystal region content in each ageing step material, first to XRD curve
The fitting of Guass swarming is carried out, the ratio that two sharp peak areas account for the spectral line gross area is calculated and obtains crystallinity, finally draw crystallization
Spend the change curve with ageing time.
Further, determine material crystalline melting enthalpy and melt initiation temperature degree with the change of ageing time in the step S6
First material is carried out when law to eliminate thermal history operation, is specifically included: being first warming up to the measurement highest temperature and keeps after a certain period of time
Room temperature is cooled to identical speed and is keeping certain time, and melting curve, melting are then obtained again with heating rate before
Enthalpy and melting temperature finally draw melting enthalpy and melting temperature with the change curve of ageing time respectively.
Further, in the step S6, need first heating material to 150 DEG C, and keep after constant temperature 5min again with 10 DEG C/
Min is cooled to room temperature, finally heats up to obtain melting curve with the speed of 10 DEG C/min.
Compared with prior art, XLPE material heat ageing dynamic process multiphase associated detecting method provided by the invention includes
Gas phase analysis, solid phase assays and the crystal phase analysis of ageing process can comprehensively reflect that the material of XLPE ageing process decomposes
Mechanism provides new approaches for the Analysis on ageing mechanism of XLPE.
Detailed description of the invention
Fig. 1 is dynamic process multiphase associated detecting method flow chart of the invention.
Fig. 2 is the FTIR spectrum curve that the XLPE sample of this invention changes with ageing time.
Fig. 3 is the sample C element content of this invention with the change curve of ageing time.
Fig. 4 is the sample O constituent content of this invention with the change curve of ageing time.
Fig. 5 is the sample H element content of this invention with the change curve of ageing time.
Fig. 6 be this invention sample difference thermal aging time under generate isobutene content change curve.
Fig. 7 is the change curve of the sample crystal region content of this invention.
Fig. 8 be respectively this invention sample crystalline fusion enthalpy and melt initiation temperature degree with ageing time change curve.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
As shown in Figure 1, a kind of heat ageing dynamic process multiphase associated detecting method of XLPE material, comprising the following steps:
S1, XLPE test piece is produced according to cable common prescription, to accelerate heat ageing process, is carried out in 160 DEG C -200 DEG C of temperature
Aging, ageing time are respectively 0h, 6h, 12h, 18h, for 24 hours and 30h, take out one group of XLPE sample and a packet gas every 6h
Body, every group of XLPE sample include 3 XLPE test pieces；Keep sample size identical, the length of the XLPE sample is generous to be respectively
30mm×30mm×1mm；
S2, after being cooled to room temperature for 24 hours, FTIR spectrum analysis is carried out to XLPE sample under each thermal aging time, is detected
The change curve of chemical group to 1-10 μm of XLPE material surface；It is main in order to describe the dynamic changing process of its degree of aging
It will be to one of the measurement index of the carbonyl peak under each different thermal aging times occurred with enhancing as degree of aging, such as Fig. 2
It is shown；
S3, the progress LIBS analysis of XLPE sample is obtained by multiple pulses laser bombardment XLPE specimen surface same position
The XLPE sample element spectrogram under different thermal aging times after preceding 30 bombardments, carries out 30 element spectrograms using entropy assessment
Mean analysis extracts the characteristic frequency spectrum peak intensity of C element, O element and H element under different thermal aging times, draws out difference
Elemental characteristic peak intensity with thermal aging time change curve, as shown in figure 3, drawing different element-intensities with the change of ageing time
It include excluding obvious errors point to be again averaging the spectral intensity of left point when changing curve graph；
S4, gas chromatographic analysis is carried out by the gas generated under the different heat ageing stages to XLPE sample, it is each in order to determine
Each characteristic peak in chromatogram need to be analyzed and be compared to the organic gas that a peak may represent, final to combine crosslinked polyethylene itself
Cross-linked structure, the top-isobutene for extracting gas chromatogram analyzed, and the isobutene under different thermal aging times is drawn
Changes of contents curve, as shown in fig. 6, first calculating the total gas of gas with various Zhan before mapping to gas content with the variation of ageing time
The ratio of body content, then ratio is drawn with the change curve of ageing time；
S5, by under different thermal aging times XLPE sample carry out XRD analysis, for quantitative analysis XLPE material crystalline degree
Variation, be fitted by Gauss swarming, calculate crystal difference crystallographic plane diffraction peak area accounting in XLPE material, obtain with old
Change the changing rule of time XLPE material crystals, specific change curve is as shown in Figure 7；
S6, by doing dsc analysis to the XLPE under different thermal aging times, first heating material is to 150 DEG C and keeps constant temperature 5min
Thermal history is eliminated, then is warming up to 150 DEG C again to room temperature with the speed decrease temperature crystalline of 10 DEG C/min, obtains the melting of XLPE material
Peak area, the variation of energy needed for characterization XLPE material crystals are melted, discloses the change of crystalline region in XLPE material from another point of view
Law, as shown in Figure 8；
S7, it is normalized to obtaining curve in described step S2, S3, S4, S5, S6, obtains each parameter with ageing time
Changing rule, to speculate the agine mechaism of XLPE material.
In the present embodiment, by carrying out FTIR spectrum analysis to sample, it can intuitively reflect its carbonyl content
Variation tendency, as shown in Fig. 2, with the increase of thermal aging time, carbonyl content is more and more.
It is respectively 0h, 6h, 12h, 18h, sample C, O, H element for 24 hours and when 30h that Fig. 3 to Fig. 5, which is in ageing time respectively,
Changes of contents curve, in 12-18h, C, O constituent content variation slope increase suddenly it can be seen from curve, and with heat
The increase of ageing time, C, O, the content of H element are increasing.
In the present embodiment, Fourier infrared spectrograph using Japanese Shimadzu Corporation IRAffinity-1S analysis, by declining
Subtract the measurement of total reflection (Attenuated Total Reflection, ATR) mode, scanning times are 20 times, resolution ratio 2cm-1, scanning range is 500-4000 cm-1。
Laser induced breakdown spectroscopy (LIBS) applies LIBS equipment --- the J200 laser spectrum of spectrum company using the U.S.
Elemental analyser.
Gas-chromatography is analyzed using the gaseous mass analyzer HP5973GCMS of hewlette-packard, mass range 1.5-
800u, scanning speed 5000-10000u/sec.
X-ray polycrystalline diffraction carries out the crystal region XRD content point using the D8 type X-ray diffractometer of Bruker company, Germany
Analysis, angular accuracy are up to 0.01 °.
Differential scanning calorimetry carries out DSC to XLPE sample using the DSC214 type differential scanning calorimeter of Nai Chi company, Germany
Experiment, each sample sampling 5mg or so, atmosphere are nitrogen, and heating rate 10K/min, temperature range is 30 DEG C -140 DEG C.
Above-described embodiment is better embodiment of the invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any not violate made changes, modifications, substitutions, combinations, simplifications under spiritual essence and principle of the invention equal
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of XLPE material heat ageing dynamic process multiphase associated detecting method, which comprises the steps of:
S1, XLPE test piece is produced according to cable common prescription, is pressed in the small-sized ageing oven of 160~200 DEG C of closing of temperature range
Setting time carries out aging, takes out one group of XLPE sample and a packet gas at regular intervals, if every group of XLPE sample includes
Dry plate XLPE test piece；
S2, it is cooled to room temperature, FTIR spectrum analysis is carried out to XLPE sample afterwards for 24 hours, obtain organic official in reflection material
It can the variation of group and the FTIR spectrum curve of degree of oxidation；
S3, by carrying out LIBS analysis to XLPE sample, extract the characteristic frequency spectrum peak intensity of C element, O element and H element, draw
Different element-intensities are made with the change curve of ageing time；
S4, by carrying out gas chromatographic analysis to the gas collected at regular intervals, determine the gas of its ageing process release
Type obtains gas content with the change curve of ageing time；
S5, XRD analysis is carried out to XLPE aged samples, determines the change curve of crystal region content in each ageing step material；
S6, dsc analysis is carried out to XLPE aged samples, determines material crystalline melting enthalpy and melt initiation temperature degree with ageing time
Change curve；
S7, it is normalized to obtaining curve in described step S2, S3, S4, S5, S6, obtains each parameter with ageing time
Changing rule, to speculate the agine mechaism of XLPE material.
2. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that step
In rapid S1, ageing time is respectively 0h, 6h, 12h, 18h, for 24 hours and 30h, takes out one group of XLPE sample and a packet every 6h
Gas, every group of XLPE sample include 3 XLPE test pieces.
3. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that institute
The generous length for the XLPE test piece stated is respectively 30mm*10mm*1mm.
4. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that step
It is specifically to calculate carbonyl bands of a spectrum related with deterioration by oxidation feature when obtaining the variation of organo-functional group in material in rapid S2
1720cm-1With the bands of a spectrum 2010cm that will not change because of hot endowmentization-1Absorbance ratio.
5. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that step
It is red using the IRAffinity-1S type Fourier transformation of Japanese Shimadzu Corporation that infrared spectrum analysis is carried out to XLPE sample in rapid S2
External spectrum instrument to sample carry out physico-chemical analysis, by decaying be all-trans emission mode measurement, scanning times be 20 times, resolution ratio 2cm-1,
Scanning range is 500~4000cm-1。
6. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that step
In rapid S3, when shown change curve for drawing different element-intensities with ageing time includes excluding obvious errors point again to residue
The step of spectral intensity of point is averaging.
7. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that step
In rapid S4, before mapping to gas content with the variation of ageing time, the ratio of the total gas content of gas with various Zhan is first calculated, then draw
Ratio processed with ageing time change curve.
8. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that step
In rapid S5, when determining the variation of crystal region content in each ageing step material, the fitting of Guass swarming, meter first are carried out to XRD curve
It calculates the ratio that two sharp peak areas account for the spectral line gross area and obtains crystallinity, it is bent with the variation of ageing time finally to draw crystallinity
Line.
9. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 1, which is characterized in that institute
State when determining the changing rule of material crystalline melting enthalpy and melt initiation temperature degree with ageing time in step S6 first to material into
Row eliminates thermal history operation, specifically includes: being first warming up to measurement highest temperature holding and is cooled to room after a certain period of time with identical speed
Temperature is keeping certain time, then obtains melting curve, melting enthalpy and melting temperature again with heating rate before, finally
Melting enthalpy and melting temperature are drawn respectively with the change curve of ageing time.
10. XLPE material heat ageing dynamic process multiphase associated detecting method according to claim 9, which is characterized in that
In the step S6, first heating material is needed to be cooled to room temperature again to 150 DEG C, and after keeping constant temperature 5min with 10 DEG C/min, finally
It heats up to obtain melting curve with the speed of 10 DEG C/min.
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| CN110579692A (en) * | 2019-09-17 | 2019-12-17 | 国网四川省电力公司电力科学研究院 | Method for rapidly measuring crosslinking degree of XLPE cable on site |
| CN110579692B (en) * | 2019-09-17 | 2021-07-06 | 国网四川省电力公司电力科学研究院 | Method for rapidly measuring crosslinking degree of XLPE cable on site |
| CN113551809A (en) * | 2020-04-23 | 2021-10-26 | 中国石油化工股份有限公司 | Memory, FTIR-based reaction thermal effect test analysis method, device and equipment |
| CN113552109A (en) * | 2020-04-23 | 2021-10-26 | 中国石油化工股份有限公司 | Memory, reaction thermal effect test analysis method, device and equipment based on Raman spectrum |
| CN113551809B (en) * | 2020-04-23 | 2023-12-05 | 中国石油化工股份有限公司 | Memory, FTIR-based reaction thermal effect test analysis method, device and equipment |
| 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 |
| CN111721624A (en) * | 2020-06-03 | 2020-09-29 | 中广核三角洲（太仓）检测技术有限公司 | Crystallinity-based nuclear power PEEK material thermal aging mechanism evaluation method |
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