CN107314942A - A kind of method of the degree of cross linking of cross-linked polrvinyl chloride after fast verification irradiation - Google Patents
A kind of method of the degree of cross linking of cross-linked polrvinyl chloride after fast verification irradiation Download PDFInfo
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/60—Investigating resistance of materials, e.g. refractory materials, to rapid heat changes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0092—Visco-elasticity, solidification, curing, cross-linking degree, vulcanisation or strength properties of semi-solid materials
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- G01N2203/02—Details not specific for a particular testing method
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- G01N2203/0226—High temperature; Heating means
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0262—Shape of the specimen
- G01N2203/0268—Dumb-bell specimens
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
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Abstract
The present invention relates to the method for the degree of cross linking of the cross-linked polrvinyl chloride after a kind of irradiation of fast verification, this method includes sample and prepares the step of being calculated with hot elongation percentage, by the corresponding size parameter for calculating dumbbell shape sample and tubulose sample, and respective samples are put into baking oven apply corresponding mechanical stress come to obtain result calculate, so as to obtain the hot elongation percentage of sample, further to verify the irradiation intensity of sample experience.The beneficial effects of the invention are as follows the degree that can grasp polyvinyl chloride irradiation dose, the size of the degree of cross linking, so that polychloroethylene insulation material is preferably applied in electric wire product design use.
Description
Technical field
The present invention relates to the method for the degree of cross linking of the cross-linked polrvinyl chloride after a kind of irradiation of fast verification, it is adaptable to which automobile is used
The checking of the degree of cross linking of cross-linked polrvinyl chloride insulated low-voltage electric.
Background technology
Polychloroethylene insulation material has the flexibility of thermoplasticity and macromolecular, and molecule, which contains chlorine atom, makes resin have hardly possible
The characteristic of combustion property and the resistance to water environment of preferable chemical resistance, by polar bond so that intermolecular active force is big, thus has
Preferable mechanical strength, it is economical and practical and performance is stable for low-voltage cable.But because molecular structure has polar group and made
Material electrical insulation capability it is not ideal enough, heat endurance is not good enough, and heat resistance is relatively low.80-85 DEG C of polychloroethylene insulation material is opened
Begin to soften, 130 DEG C start to decompose, and used in cable insulation material, when cable may rise by current temperature, are subjected to electrically and thermally
Material softening deformation, degraded can be made under effect, so as to cause electrical insulation properties to reduce.Cross-linked polrvinyl chloride after irradiation has
Excellent electrical insulation properties, its heat-resisting and mechanical performance is greatly improved, and overcomes the shortcoming of polyvinyl chloride insulation.Irradiation
Dosage is small, and crosslink material degree is small, it is impossible to reach heat-resisting and mechanical performance raising, it is impossible to meet product requirement, irradiation dose mistake
Height, the degree of cross linking is excessive, and mechanical strength and hardness can be caused all to increase again, therefore, to crosslinking in electric wire production
The detection control of the degree of cross linking of insulating materials is a very important step.Cross-linked polrvinyl chloride heat extension after test irradiation
Rate can quickly verify its degree of cross linking, and the size of the degree of cross linking directly affects electric wire performance, such as light, heat and the mechanicalness of electric wire
Energy.Most of materials have the treatment conditions and technological parameter of corresponding hot elongation percentage test in product in the prior art, right
Performing discovery according to existing hot elongation percentage treatment conditions and technological parameter in the cross-linked polrvinyl chloride insulating materials after irradiation can not
Proper testing is carried out to sample, therefore the degree of cross linking of the cross-linked polrvinyl chloride insulating materials after irradiation can not be verified.Currently without
It is related to the prior art that hot elongation percentage test is carried out to the product of the polyvinyl chloride cable after irradiation.
The method for testing the degree of cross linking in the prior art, main is exactly by chemical extraction mode calculated for gel rate, experiment step
Suddenly it is:Dry and --- weigh and --- extract --- drying --- to weigh, by the weight of sample before and after extraction, calculated for gel contains
Amount, determines the degree of cross linking, and the method completes once to test at least to need 72 hours, can accurately judge the degree of cross linking, but the cycle compared with
It is long.
The content of the invention
It is an object of the invention to provide a kind of fast verification by testing the hot elongation percentage of crosslinked polyethylene after irradiation
The method of the degree of cross linking of cross-linked polrvinyl chloride after irradiation, so that the irradiation dose of control cross-linked polrvinyl chloride is obtained or reaches,
Efficiently control the purpose of the optimum performance of product.The hot elongation percentage test of the present invention, being prepared into end test from sample only needs
Want 1h, the test period is short, can qualitatively preliminary fast verification irradiation dose (or degree of cross linking) size.
To reach above-mentioned purpose, the present invention uses following technical proposals:
A kind of method of the degree of cross linking of cross-linked polrvinyl chloride after fast verification irradiation, this method includes step:
(1) prepared by sample
Three samples of every at least 100mm length are prepared from sample, are deposited at least at room temperature (23 ± 5) DEG C
3h, wherein insulating bore are tubulose sample when being less than 5mm, and insulating bore, which is equal to or more than cut vertically during 5mm, is formed as mute
Bell type sample, wherein dumbbell shape sample should be produced after all convex ridges of removing and/or semi-conductive layer from insulation and sheath internal layer,
Two markings are put in the middle part of dumbbell shape sample;
I. for dumbbell shape sample
A. insulation sample should be polished or scabbled, and the sample between two mark lines is had parallel surface;
B. the width of each sample is measured, minimum value is taken as the width of this group of dumbbell shape sample;
C. taken in each sample thickness and its thickness is measured in stretch zones, take minimum value as the thickness of this group of dumbbell shape sample
Degree;
II. for tubulose sample
A. the conductor of each sample is taken out, the accurate remaining insulated lengths 100mm of measurement sample, in the sample between mark two
Bar markings, and respectively insert at sample two ends a bit of metal needle tubing less than sample internal diameter, the upper and lower ends meeting of tubulose sample
It is jammed and is put into baking oven, two ends, which can soften, under conditions of heating can form closing space inside tubular specimen, in heating
Under conditions of can expand, therefore two ends respectively insertion less than internal diameter metal needle tubing, discharge internal gas;
B. the external diameter of sample is measured;
C. the half of the thickness, the i.e. difference of external diameter and internal diameter of sample is measured;
(2) hot elongation percentage is calculated
A. the sample prepared is suspended on test temperature in 200 ± 3 DEG C of ageing ovens, sample bears machinery should
Power:4N/cm2, i.e. 4MPa, sample following folder weight, load weight calculation formula is as follows:
Sectional area A (the mm of dumbbell shape sample2)=specimen width mm × thickness mm
Sectional area A (the mm of tubulose sample2)=π (D- δ) δ
Load weight M (g)=A/100 × 0.102 × 1000 × 4=4.08A
In formula:D:External diameter mm δ:Thickness;
B. when oven temperature goes back up to test temperature, test specimen is placed to be kept after 10min again in baking oven, measurement markers line spacing
From length and hot elongation percentage is calculated, calculation formula is as follows:
Sample marking is long before hot elongation percentage %=(sample marking length before sample marking length-heating after heating)/heating
Degree × 100%;
C. sample is stayed in from releasing pulling force on test specimen and taken after recovering 5min under the test temperature in ageing oven from baking oven
Go out test specimen, be slowly cooled to room temperature, again the distance between measurement markers line.Examining the result of hot elongation percentage needs two parameters,
One:Elongation under high-temperature cabinet internal load;Two:The elongation after load cooling is removed under high temperature.Therefore measurement markers line again
Between distance be exactly the calculative value of second point parameter.
After the result of hot elongation percentage of test specimen is obtained, the size of the degree of cross linking qualitatively can be tentatively judged.
Wherein the distance of two markings of dumbbell shape sample and tubulose sample is 20mm.
Wherein the width determination mode of dumbbell shape sample measures its width to be taken respectively on three samples at three, calculates flat
Minimum average B configuration value in average, three specimen width average datas is the width of this group of dumbbell test specimen.
Wherein the thickness determination mode of dumbbell shape sample measures it to be taken respectively at three in the stretch zones of three samples
Thickness, calculates thickness of the minimum average B configuration value in average value, three sample thickness average datas for this group of dumbbell test specimen.
The thickness of wherein each dumbbell shape sample should be not less than 0.6mm, preferably not less than no more than 2.0mm, 0.8mm, no
More than 2.0mm.
The external diameter determination mode of wherein described tubulose sample is that sample is intercepted on sample and measurement position is marked, and is put
Put on detection device, being mutually perpendicular to both direction in measurement position mark measures its external diameter, calculate being averaged for two data
It is worth the external diameter as tubulose sample.
Insulation is cut into by the thickness determination mode of wherein described tubulose sample to intercept sample on sample with blade
Thin slice, is placed on detection device, six points for taking thickness minimum in a circumferential direction, measures the thickness value at the two points,
The average value for calculating this six data is used as the thickness of tubulose sample.
Wherein in the b step of the hot elongation percentage calculation procedure, oven temperature goes back up to the time control of test temperature
Within 5min.Baking oven needed when reaching and sample is placed after temperature it is quick, from without causing oven temperature to be greatly lowered, if
Temperature reduction is excessive, will be unable to meet the condition that sample is tested under conditions of 200 ± 3 DEG C, illustrates:Temperature is reduced to 150 DEG C,
Now sample is put 10min in baking oven into and just recovered to 200 DEG C, and sample, which may have, necessarily extends phenomenon, but is not requirement
200 degrees celsius under, if start timing 10min, equivalent to sample under the conditions of 150-200 DEG C and 200 DEG C two
Elongation, the result now measured is inaccurate, therefore set point of temperature is gone up the time, and reaching can be true when time different people is operated each time
Protect the accurate of measurement result.
Wherein in the b step of the hot elongation percentage calculation procedure, should be dried apart from length opening between measurement markers line
Measurement is finished in chamber door 30s.Elongation under high temperature is measured in measuring method needs door of unpacking, and case internal-external temperature difference is big, can make temperature
Rapidly lower, cause sample because by temperature change, shrinkage phenomenon occurs in sample, causes measurement data inaccurate, therefore need
Ensuring measuring speed, The faster the better.If equipment can meet door of not unpacking, from observation window outside, direct measurement data can be ignored
The requirement of measurement in 30s.
Beneficial effect acquired by the present invention is:Can fast verification polyvinyl chloride irradiation dose size, so as to preliminary
Obtain the degree of cross linking of cross-linked polrvinyl chloride insulating materials, it is ensured that product use requirement.
Brief description of the drawings
In order to be easier to understand technical scheme and beneficial technique effect, by referring to what is be shown in the drawings
The present invention is described in detail the embodiment of the present invention.These accompanying drawings depict only typical case's implementation of the present invention
Mode, does not constitute the limitation to protection scope of the present invention, wherein:
Fig. 1 is the outline drawing of dumbbell shape sample.
Fig. 2 and Fig. 3 are tubulose sample thickness instrumentation plans.
Embodiment
The method that the present invention proposes a kind of degree of cross linking of the cross-linked polrvinyl chloride after fast verification irradiation, this method includes
Once step:
(1) prepared by sample
Three samples of every at least 100mm length are prepared from sample, are deposited at least at room temperature (23 ± 5) DEG C
3h, wherein insulating bore are tubulose sample when being less than 5mm, and insulating bore, which is equal to or more than cut vertically during 5mm, is formed as mute
Bell type sample, wherein dumbbell shape sample should be produced after all convex ridges of removing and/or semi-conductive layer from insulation and sheath internal layer,
Two markings are put in the middle part of dumbbell shape sample, the distance of two markings is 20mm;
I. for dumbbell shape sample (its profile is as shown in fig. 1)
A. insulation sample should be polished or scabbled, and the sample between two mark lines is had parallel surface;
B. the width of each sample is measured, minimum value is taken as the width of this group of dumbbell shape sample, if tried dumbbell shape
The width uniformity of sample leaves a question open, and can respectively be taken on three samples and its width is measured at three, calculates average value, and three samples are wide
The minimum average B configuration value spent in average data is the width of this group of dumbbell test specimen;
C. taken in each sample thickness and its thickness is measured in stretch zones, take minimum value as the thickness of this group of dumbbell shape sample
Degree, if left a question open to the thickness evenness of dumbbell shape sample, can respectively take in the stretch zones of three samples and be measured at three
Its thickness, calculates thickness of the minimum average B configuration value in average value, three sample thickness average datas for this group of dumbbell test specimen, its
In the thickness of each dumbbell shape sample should be not less than 0.6mm, no more than no more than 2.0mm, preferably not less than 0.8mm, 2.0mm;
II. for tubulose sample
A. the conductor of each sample is taken out, the accurate remaining insulated lengths 100mm of measurement sample, in the sample between mark two
Bar markings, the distance of two markings is 20mm, and respectively inserts at sample two ends a bit of metal needle less than sample external diameter
Pipe;
B. the external diameter of sample is measured, the external diameter determination mode of the tubulose sample is that sample is intercepted on sample and is marked
Remember measurement position, be placed on detection device, being mutually perpendicular to both direction in measurement position mark measures its external diameter, calculates two
The average value of individual data as tubulose sample external diameter;
C. the half of the thickness, the i.e. difference of external diameter and internal diameter of sample is measured, wherein the thickness determination side of the tubulose sample
Insulation is thinly sliced, is placed on detection device, taken in a circumferential direction to intercept sample on sample by formula with blade
Six minimum points of thickness, measure the thickness value at the two points, calculate the average value of this six data as tubulose sample
Thickness, as shown in Figures 2 and 3;
(2) hot elongation percentage is calculated
A. the sample prepared is suspended on test temperature in 200 ± 3 DEG C of ageing ovens, sample bears machinery should
Power:4N/cm2, i.e. 4MPa, sample following folder weight, load weight calculation formula is as follows:
Sectional area A (the mm of dumbbell shape sample2)=specimen width mm × thickness mm
Sectional area A (the mm of tubulose sample2)=π (D- δ) δ
Load weight M (g)=A/100 × 0.102 × 1000 × 4=4.08A
In formula:D:External diameter mm δ:Thickness;
B. when oven temperature goes back up to test temperature (preferably within 5min), test specimen is placed in baking oven and keeps 10min again
Afterwards, measurement markers wire spacing length and hot elongation percentage is calculated, should be finished opening measure in oven door 30s, calculation formula is such as
Under:
Sample marking is long before hot elongation percentage %=(sample marking length before sample marking length-heating after heating)/heating
Degree × 100%;
C. sample is stayed in from releasing pulling force on test specimen and taken after recovering 5min under the test temperature in ageing oven from baking oven
Go out test specimen, be slowly cooled to room temperature, again the distance between measurement markers line.
Testing experiment one
Listed in following table when tubulose sample is identical in the time with dumbbell shape sample after identical irradiation intensity irradiates, it is different
Heat extensibility energy under test temperature and different mechanical stresses.It can be seen that test temperature is at 200 degrees Celsius from the table, machinery
Stress under 4MPa can test result effectively, by the experiment determine the present invention test temperature and experiment in the machinery that applies
Stress.
Testing experiment two
Synthermal, the equivalent time such as list after the irradiation of identical irradiation intensity in following table, different mechanical stresses, difference is led
Under conditions of body section size, the heat extensibility energy of sample, every kind of condition test sample is three, the test number more than
According to none sample passes through experiment during mechanical stress >=7.5MPa;As mechanical stress≤2MPa for cross-sectional area of conductor sample less than normal
Product are due to applying underload, it is impossible to weigh weight and complete experiment;It is desirable result to select 5MPa or 4MPa.
Testing experiment three
Examination under conditions of same equitemperature, equivalent assay time, equal mechanical stress, different irradiation doses is demonstrated in following table
The hot extension situation of sample, former irradiation dose is No. 1 sample, and No. 2 sample irradiation dosage increase 0.3Mrad, 3, No. 4 samples are with such
Push away., can be complete for the sample of the different irradiation doses of zone of reasonableness when understanding mechanical stress from the data that following table is listed for 4MPa
Into testing out, while different irradiation doses can also tell the difference of test result.
Testing experiment four
Examination under conditions of same equitemperature, equivalent assay time, equal mechanical stress, different irradiation doses is demonstrated in following table
The hot extension situation of sample, former irradiation dose is No. 1 sample, and No. 2 sample irradiation dosage increase 0.3Mrad, 3, No. 4 samples are with such
Push away.When understanding mechanical stress from the data that following table is listed for 5MPa, the hot extension value of sample is bigger than normal, while sample occurs in indirect
Phenomenon of rupture, experimental result is unstable, there is shortcoming
The present invention can be embodied in other specific forms, but this is without departing from protection scope of the present invention, sheet
The protection domain of invention is defined only by the following claims.
Claims (9)
1. a kind of method of the degree of cross linking of the cross-linked polrvinyl chloride after fast verification irradiation, this method comprises the following steps:
(1) prepared by sample
Three samples of every at least 100mm length are prepared from sample, at least 3h is deposited at room temperature (23 ± 5) DEG C, its
Middle insulating bore is tubulose sample when being less than 5mm, and insulating bore, which is equal to or more than cut vertically during 5mm, is formed as dumbbell shape examination
Sample, wherein dumbbell shape sample should be produced after all convex ridges of removing and/or semi-conductive layer from insulation and sheath internal layer, in dumbbell shape
Two markings are put in the middle part of sample;
I. for dumbbell shape sample
A. insulation sample should be polished or scabbled, and the sample between two mark lines is had parallel surface;
B. the width of each sample is measured, minimum value is taken as the width of this group of dumbbell shape sample;
C. taken in each sample thickness and its thickness is measured in stretch zones, take minimum value as the thickness of this group of dumbbell shape sample;
II. for tubulose sample
A. the conductor of each sample is taken out, the accurate remaining insulated lengths 100mm of measurement sample, in the sample between two marks of mark
Will line, and respectively insert at sample two ends a bit of metal needle tubing less than sample external diameter;
B. the external diameter of sample is measured;
C. the half of the thickness, the i.e. difference of external diameter and internal diameter of sample is measured;
(2) hot elongation percentage is calculated
A. the sample prepared is suspended on test temperature in 200 ± 3 DEG C of ageing ovens, sample bears mechanical stress:4N/
cm2, i.e. 4MPa, sample following folder weight, load weight calculation formula is as follows:
Sectional area A (the mm of dumbbell shape sample2)=specimen width mm × thickness mm
Sectional area A (the mm of tubulose sample2)=π (D- δ) δ
Load weight M (g)=A/100 × 0.102 × 1000 × 4=4.08A
In formula:D:External diameter mm δ:Thickness;
B. when oven temperature goes back up to test temperature, test specimen is placed to be kept after 10min again in baking oven, and measurement markers wire spacing is long
Spend and calculate hot elongation percentage, calculation formula is as follows:
The preceding sample marking length of hot elongation percentage %=(sample marking length before sample marking length-heating after heating)/heating ×
100%;
C. sample is stayed under the test temperature in ageing oven from releasing pulling force on test specimen and recovers to take out examination after 5min from baking oven
Part, is slowly cooled to room temperature, again the distance between measurement markers line.
2. according to the method described in claim 1, the distance of wherein two markings of dumbbell shape sample and tubulose sample is
20mm。
3. according to the method described in claim 1, wherein the width determination mode of dumbbell shape sample is to distinguish on three samples
Take and its width is measured at three, it is this group of dumbbell examination to calculate the minimum average B configuration value in average value, three specimen width average datas
The width of part.
4. according to the method described in claim 1, wherein the thickness determination mode of dumbbell shape sample is the stretching in three samples
Taken respectively in region and its thickness is measured at three, the minimum average B configuration value calculated in average value, three sample thickness average datas is
The thickness of this group of dumbbell test specimen.
5. according to the method described in claim 1, it is not more than wherein the thickness of each dumbbell shape sample should be not less than 0.6mm
2.0mm, preferably not less than 0.8mm, no more than 2.0mm.
6. according to the method described in claim 1, wherein the external diameter determination mode of the tubulose sample is to be cut on sample
Materials and mark measurement position, be placed on detection device, being mutually perpendicular to both direction in measurement position mark measures it
External diameter, the average value for calculating two data is used as the external diameter of tubulose sample.
7. according to the method described in claim 1, wherein the thickness determination mode of the tubulose sample is to be cut on sample
Materials, thinly sliced insulation with blade, be placed on detection device, six points for taking thickness minimum in a circumferential direction,
The thickness value at the two points is measured, the average value for calculating this six data is used as the thickness of tubulose sample.
8. according to the method described in claim 1, wherein in the b step of the hot elongation percentage calculation procedure, oven temperature is returned
The time control of test temperature is raised within 5min.
9. the method according to any one of claim 1-8, wherein in the b step of the hot elongation percentage calculation procedure,
Should be finished apart from length opening to measure in oven door 30s between measurement markers line.
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Cited By (2)
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CN111366459A (en) * | 2020-03-27 | 2020-07-03 | 威海联桥新材料科技股份有限公司 | Method for testing crosslinking degree of crosslinked polyethylene |
WO2023019721A1 (en) * | 2021-08-19 | 2023-02-23 | 深圳供电局有限公司 | Cross-linking performance consistency characterization method for cross-linked polyethylene 500 kv cable insulation material |
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WO2023019721A1 (en) * | 2021-08-19 | 2023-02-23 | 深圳供电局有限公司 | Cross-linking performance consistency characterization method for cross-linked polyethylene 500 kv cable insulation material |
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