CN113008932A - Method for correcting cross-linking degree test error - Google Patents
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- 238000012360 testing method Methods 0.000 title claims abstract description 180
- 238000004132 cross linking Methods 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000000605 extraction Methods 0.000 claims abstract description 57
- 238000000113 differential scanning calorimetry Methods 0.000 claims abstract description 46
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000004073 vulcanization Methods 0.000 claims abstract description 36
- 239000008096 xylene Substances 0.000 claims abstract description 35
- 239000002313 adhesive film Substances 0.000 claims abstract description 32
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000012937 correction Methods 0.000 claims abstract description 9
- 238000005070 sampling Methods 0.000 claims abstract description 6
- 238000003475 lamination Methods 0.000 claims description 19
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- 238000012545 processing Methods 0.000 claims description 3
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- 238000010030 laminating Methods 0.000 description 2
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000005001 laminate film Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
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Abstract
The invention discloses a method for correcting cross-linking degree test errors, which comprises the steps of firstly sampling at different positions of the same laminated adhesive film to obtain a test total sample, dividing the test total sample into a sample A and a sample B, and dividing an adhesive film which is not laminated into a sample C and a sample D; respectively preparing a sample A, a sample B, a sample C and a sample D, testing the sample A and the sample C after sample preparation by using a differential scanning thermal method, testing the sample B after sample preparation by using a xylene extraction method, and testing the sample D after sample preparation by using a differential scanning thermal method after vulcanization test; calculating the degree of crosslinking G according to the result obtained after the sample B is completely extracted by a xylene extraction method6Calculating the degree of crosslinking G according to the result obtained by performing differential scanning calorimetry test on the sample D after the vulcanization test7(ii) a The degree of crosslinking G is calculated6Degree of crosslinking G7And linear correction relation therebetween. By using the invention, the test error can be reduced and the test efficiency can be improved.
Description
Technical Field
The invention relates to the field of photovoltaic module assembly, in particular to a method for testing a crosslinking degree.
Background
EVA adhesive films and POE adhesive films are thermosetting packaging materials commonly used in the photovoltaic industry, and the EVA adhesive films are prepared by adding various additives such as coupling agents, initiators, antioxidants and the like into EVA resin (copolymer of ethylene and vinyl acetate). The POE adhesive film is prepared by adding various additives such as a coupling agent, an initiator, an antioxidant and the like into an ethylene-alpha-olefin copolymer serving as a matrix. When the EVA adhesive film and the POE adhesive film are heated to a certain temperature, the cross-linking agent can be decomposed to generate free radicals so as to initiate the combination between EVA molecules and POE molecules, and a cross-linking reaction is carried out to form a three-dimensional network structure so as to enable the EVA molecules and the POE molecules to be cured and cross-linked.
The crosslinking degree is the mass ratio of linear molecules to reticular molecules when the adhesive film is heated, and is a physical quantity used for representing the crosslinking degree of EVA and P OE, the crosslinking degree not only determines the mechanical properties such as the peeling strength, the tensile strength and the like of the cured EVA adhesive film and the POE adhesive film, but also influences the external environment aging performance of the photovoltaic module, plays a crucial role in the service life and the quality of the photovoltaic module, and generally, the crosslinking degree of the adhesive film is preferably 75-90%.
At present, the common method for testing the crosslinking degree of EVA and POE adhesive films in the photovoltaic industry is chemical method-xylene extraction and differential scanning heat test. The chemical extraction method contains more uncertain factors (human, instrument, environment and the like) which can cause errors in the degree of crosslinking, so that the judgment of the mechanical property and the aging property test of the photovoltaic module is influenced, and the differential scanning heat test method can cause errors in the degree of crosslinking due to uncertain factors such as uneven lamination temperature and the like.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to solve the technical problems that the testing time is longer when the cross-linking degree is tested by the chemical method at present, and the testing error is larger due to more interference factors, the invention provides a method for correcting the testing error of the cross-linking degree, which combines the vulcanization test and the differential scanning heat test together, thereby not only saving the testing time, but also reducing the influence of human factors on the testing result.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method of correcting cross-linking degree test errors, comprising the steps of:
s11: sampling at different positions of the same laminated adhesive film to obtain a total test sample, dividing the total test sample into a sample A and a sample B, and dividing an un-laminated adhesive film into a sample C and a sample D;
s12: respectively preparing the sample A, the sample B, the sample C and the sample D, testing the sample A and the sample C after sample preparation by using a differential scanning thermal method, testing the sample B after sample preparation by using a xylene extraction method, testing the sample D after sample preparation by using a first vulcanization test, and testing the sample D after the vulcanization test by using a differential scanning thermal method;
s13: calculating the degree of crosslinking G according to the data obtained after the sample B is completely extracted by a xylene extraction method6Calculating the crosslinking degree G according to data obtained by performing differential scanning calorimetry test on the sample D after the vulcanization test7(ii) a According to the relative error calculation formula (G)7-G6)/G7X 100% calculation of the degree of crosslinking G6With the degree of crosslinking G7Relative error therebetween;
s14: repeating the calculation process of step S13 to obtain a plurality of relative errors; analyzing according to the relative errors to obtain the crosslinking degree G6With the degree of crosslinking G7The correction relation is linear relation.
By adopting the method, on one hand, the test error caused by uneven lamination temperature to differential scanning heat test can be reduced, on the other hand, the usage amount of the adhesive film during the detection of the crosslinking degree can be saved, and the waste of the adhesive film is reduced.
In an embodiment of the present invention, the modified relation is: g6＝(1-5.8％)×G7。
By adopting the method, the crosslinking degree obtained by differential scanning calorimetry is directly converted into the crosslinking degree obtained by a xylene extraction method through a correction relational expression, so that the test time is saved, and the reliability of test data can be improved.
In an embodiment of the present invention, the total test sample is a sum of samples taken from four sides and a center of the same laminated adhesive film.
By adopting the above method, the test sample can be made to have uniformity.
In an embodiment of the present invention, the sample preparation in step S12 includes:
weighing the sample A and the sample C, wherein the total mass of each sample is in the range of 7-10 mg;
taking 460 grams of the sample B and cutting it into a number of 2mm by 2mm particles;
the sample D was cut into several 30mm by 30mm samples.
By adopting the method, the subsequent test can be more convenient and faster.
In an embodiment of the present invention, the differential scanning calorimetry test in step S12 includes the following steps:
s21: opening the differential scanning calorimeter, setting parameters, adopting a program to heat up, and controlling the heating rate to be 8-12K/mi n;
s22: respectively placing the sample A and the sample C after sample preparation in test crucibles, uniformly contacting the bottom of each test crucible, respectively placing the two test crucibles in two furnaces, closing the furnace covers, and testing for 20-30 minutes;
s23: after the test is finished, taking out the test crucible in the furnace, and processing the differential scanning thermal curve to obtain test data;
s24: calculating the crosslinking degree G of the obtained test data according to a formula7。
In an embodiment of the present invention, the cross-linking degree calculation formula in step S24 is: g7＝(H1-H2) /H1X 100%, wherein, H1Denotes the heat-release enthalpy, H, of the unlaminated sample2Indicating the exothermic enthalpy of the lamination sample.
In an embodiment provided by the present invention, the xylene extraction test in step S12 includes the following steps:
s31: cleaning stainless steel wire mesh bag, oven drying, and weighingThe weight of the mesh bag is W1Respectively putting the sample B after sample preparation into five net bags, respectively sealing the bag openings to prepare sample bags, and weighing the sample bags, wherein the weight of each sample bag is W2；
S32: putting the five sample bags into a boiling dimethylbenzene solvent for extraction, wherein the extraction time is set to be 5 hours, immediately putting the sample bags into a vacuum oven after the extraction is finished, setting the temperature of the oven to be 130 ℃, and drying for 4 hours;
s33: taking the five sample bags out of the vacuum oven, cooling and weighing, wherein the weight of the extracted sample bags is W3；
S34: the weight W obtained by the test1、W2And W3The degree of crosslinking G is calculated according to the formula6。
In an embodiment of the present invention, the cross-linking degree calculation formula in step S34 is: g6＝(W3-W1)/(W 2-W1)×100％。
In an embodiment of the present invention, the parameters of the vulcanization test in the step S13 are set to be the same as the lamination parameters of the laminator.
By adopting the method, the test error caused by inaccurate lamination temperature due to large lamination area and laminator table oil or electric heating can be reduced.
The invention has the beneficial effects that: the crosslinking degree obtained by combining a vulcanization test and a differential scanning calorimetry is compared and analyzed with the crosslinking degree obtained by a chemical xylene extraction test, an error is calculated, a linear relation can be obtained, and the crosslinking degree obtained by the differential scanning calorimetry can be quickly converted into the crosslinking degree obtained by the chemical xylene extraction through the linear relation. On one hand, the invention can reduce the test error caused by the uneven lamination temperature to the differential scanning heat test; on the other hand, the usage amount of the adhesive film during the detection of the crosslinking degree can be saved, the waste of the adhesive film is reduced, the test time is saved, and the accuracy of the test result is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flowchart of a method for correcting cross-linking test errors according to an embodiment of the present invention;
FIG. 2 is a flow chart of a differential scanning calorimetry test provided in accordance with one embodiment of the present invention;
FIG. 3 is a flow chart of xylene extraction testing provided by one embodiment of the present invention;
table 1 shows the results of differential scanning calorimetry on samples a and C according to an embodiment of the present invention;
table 2 shows the test results of sample B extracted by the xylene extraction method in one step according to an embodiment of the present invention;
table 3 shows the test results of sample B obtained after secondary extraction by a xylene extraction method according to an embodiment of the present invention;
table 4 shows the test results of sample B extracted three times by the xylene extraction method according to an embodiment of the present invention;
table 5 shows the results of differential scanning calorimetry on sample D according to an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention. Furthermore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Differential Scanning Calorimetry (DSC) is a technique for measuring the power difference and temperature between a reference material and a substance to be measured at a programmed temperature. Differential scanning calorimetry has both compensated and thermal flow. In the differential scanning calorimetry, the curve of the quantity of heat applied per unit time necessary to maintain the temperature difference between the sample and the reference at zero is a DSC curve. The vertical axis of the graph represents the amount of heat applied per unit time, and the horizontal axis represents temperature or time. The area of the curve is proportional to the change in enthalpy. The differential scanning calorimeter used in the present embodiment may be, for example, a Chip-DSC-100 type differential scanning calorimeter.
The extraction method is an operation method for extracting a solute from a solution consisting of another solvent by using one solvent by utilizing the difference of the solubility of the solute in the solvents which are not mutually soluble. The solvent used in this embodiment may be, for example, a xylene solution.
The vulcanization is also called as cross-linking and curing, and the linear macromolecules are converted into a three-dimensional network structure under the conditions of certain temperature and pressure by adding a cross-linking auxiliary agent such as a vulcanizing agent, an accelerator and the like into a sample. The vulcanization instrument is an instrument for continuously measuring various performance changes in the vulcanization process of the rubber material, and the working principle of the instrument is to measure the change of the shear modulus of the rubber material in the vulcanization process, wherein the shear modulus is in direct proportion to the crosslinking density, so that the measurement result reflects the change of the crosslinking degree of the rubber material in the vulcanization process, and important parameters such as the initial viscosity, the scorching time, the vulcanization speed, the normal vulcanization time, the over-vulcanization reversion property and the like of the rubber material can be measured. The vulcanizer used in the present embodiment may be, for example, a rotorless vulcanizer (TY-6002).
Lamination refers to a molding process in which multiple layers of the same or different materials are integrally combined under heat and pressure. Different lamination temperatures have different effects on the degree of crosslinking of the adhesive film during the lamination operation. The laminator used in this embodiment may be, for example, a high temperature vacuum laminator (WD-40 TZ-H).
Referring to fig. 1, the present invention provides a method for correcting a cross-linking degree test error, comprising the following steps:
s11: sampling is carried out at different positions of the same laminated adhesive film to obtain a total test sample, the total test sample is divided into a sample A and a sample B, and one part of the non-laminated adhesive film is divided into a sample C and a sample D.
It should be noted that, in this embodiment, the test total sample includes the sum of the samples taken at the four sides and the center of the laminated adhesive film, so that the test sample has uniformity. The samples a and B each contained five test samples corresponding to the sampling positions of the laminate films. For comparative experiments, sample D was also divided into five test samples and sample C was taken. Five test samples were included in each of samples A, B, D for comparative experiments, and sample C was used to measure the exothermic enthalpy of heat for the unlaminated sample.
S12: respectively preparing a sample A, a sample B, a sample C and a sample D, testing the sample A and the sample C after sample preparation by using a differential scanning calorimetry method, testing the sample B after sample preparation by using a xylene extraction method, testing the sample D after sample preparation by first performing a vulcanization test, and then testing the sample D after the vulcanization test by using a differential scanning calorimetry method.
It should be noted that, the sample preparation of the sample a and the sample C includes weighing the sample mass, the total mass of each sample is controlled within the range of 7-10 mg, and the mass error of each sample does not exceed 5%, so that the test error caused by the mass error to the test can be reduced. 460 g of sample B is cut into a plurality of particles of 2mm by 2mm, and the test error can be reduced by cutting into the particles. Sample D was cut into several 30mm by 30mm samples, each sample having a mass of about 3 g. And after sample preparation is finished, respectively carrying out differential scanning calorimetry test on the sample A and the sample C, carrying out xylene extraction test on the sample B, and carrying out vulcanization test on the sample D. In this example, the effect of the vulcanization test is to allow crosslinking to occur in samples that have not been laminated.
S13: calculating the degree of crosslinking G according to the data obtained after the sample B is completely extracted by a xylene extraction method6Calculating the crosslinking degree G according to data obtained by performing differential scanning calorimetry test on the sample D after the vulcanization test7(ii) a According to the relative error calculation formula (G)7-G6)/G7X 100% calculation of the degree of crosslinking G6With the degree of crosslinking G7Relative error therebetween.
Referring to fig. 2, in the present embodiment, the differential scanning calorimetry test includes the following steps:
s21: opening the differential scanning calorimeter, setting parameters, adopting a program to heat up, and controlling the heating rate to be 8-12K/mi n;
s22: respectively placing the sample A and the sample C after sample preparation in test crucibles, uniformly contacting the bottom of each test crucible, respectively placing the two test crucibles in two furnaces, closing the furnace covers, and testing for 20-30 minutes;
s23: after the test is finished, taking out the test crucible in the furnace, and processing the differential scanning thermal curve to obtain test data;
s24: test data obtainedThe degree of crosslinking G is calculated according to the formula7。
In the embodiment, the sample is uniformly contacted with the bottom of the crucible, so that the test error can be reduced, and the drift of the baseline of the test result can be reduced by controlling the temperature rise rate to be 8-12K/min. The calculation formula of the DSC crosslinking degree is as follows: g7＝(H1-H2)/ H1X 100%, wherein, H1Denotes the heat-release enthalpy, H, of the unlaminated sample2Indicating the exothermic enthalpy of the lamination sample. The test results are shown in table 1, and the exothermic enthalpy of the sample C obtained by the test is 7.247J/g, that is, the exothermic enthalpy of the non-laminated sample is 7.247J/g, and the exothermic enthalpies of the five test samples of the laminated adhesive film sample a are respectively: 7.484J/g, 8.470J/g, 8.322J/g, 8.716J/g and 8.891J/g, it can be found that the enthalpy of the laminated adhesive film sample A directly subjected to DSC test is higher than that of the non-laminated sample C, which is probably caused by the non-uniform laminating temperature of the laminator.
TABLE 1 results of the experiments on the different samples tested by DSC
Referring to fig. 3, in the present embodiment, the xylene extraction test performed on sample B includes the following steps:
s31: cleaning, drying and weighing a stainless steel wire mesh bag, wherein the weight of the mesh bag is W1Respectively putting the samples B into five mesh bags, respectively sealing the bag openings to prepare sample bags, weighing, wherein the weight of each sample bag is W2；
S32: putting the five sample bags into a boiling dimethylbenzene solvent for extraction, wherein the extraction time is set to be 5 hours, immediately putting the sample bags into a vacuum oven after the extraction is finished, setting the temperature of the oven to be 130 ℃, and drying for 4 hours;
s33: packaging the sampleTaking out the sample bag from the empty oven, cooling, weighing, and weighing the sample bag after extraction, wherein the weight of the sample bag is W3；
S34: the weight W obtained by the test1、W2And W3The degree of crosslinking G is calculated according to the formula6。
In this example, xylene solvent was used to extract the uncrosslinked portion of the sample, and the degree of xylene-extracted crosslinking was calculated as: g6＝(W3-W1)/(W2-W1) X 100%, performing DSC test and xylene extraction test again on the residual sample after extraction, and repeating the steps of S31-S34 until the weight of the sample package after extraction is kept unchanged. As shown in tables 2 to 4, in this example, after three xylene extraction experiments, it is found that the weight of the sample package after extraction does not change any more, and a DSC test is performed on the residual sample after each extraction, so that it can be more intuitively found whether the uncrosslinked portion of the sample has been completely extracted, for example, the sample after three extractions has been completely extracted as indicated by no crosslinking reaction peak after the DSC test. Degree of crosslinking G of five test samples of sample B after three xylene extractions678.43%, 80.39%, 81.55%, 81.55% and 82.35% respectively.
TABLE 2 Experimental results after one-time extraction of different samples
TABLE 3 results of the experiments after the second extraction of different samples
TABLE 4 results of the experiments after three extractions of different samples
It should be noted that the direct DSC measurement of laminate sample a resulted in undesirable results, which may be due to non-uniform lamination temperature of the laminator. Therefore, the invention carries out the vulcanization test before the DSC test of the non-laminated sample, so that the sample is crosslinked, and the parameter of the vulcanization test is set to be the same as the lamination parameter of the laminator, thereby not only achieving the purpose of crosslinking the sample, but also reducing the test error caused by inaccurate lamination temperature due to larger lamination area and laminator table oil or electric heating. The DSC test procedure of the vulcanized sample is the same as that of steps S21-S24. The results are shown in table 5, and the enthalpy of heat release measured for five test samples of sample D after vulcanization are: 1.212J/G, 1.062J/G, 0.973J/G, 0.911J/G, calculated Cross-linking degree G7Respectively as follows: 83.27%, 85.35%, 86.57%, 86.58%, 87.43%. It was found that the degree of crosslinking of the unlaminated sample after the vulcanization test and the DSC test was satisfactory.
TABLE 5 results of DSC measurements of various samples after vulcanization tests
S14: repeating the calculation process of step S13 to obtain a plurality of relative errors; and analyzing according to the relative errors to obtain a correction relation between the crosslinking degree G6 and the crosslinking degree G7, wherein the correction relation is linear.
It should be noted that, the calculation process of step S13 is repeated, and the measured degree of crosslinking G after complete extraction by xylene extraction is repeated for a plurality of times6And a degree of crosslinking G obtained by DSC test after vulcanization test7Error calculation is carried out, and the cross-linking degree deviation between the two is respectively found as follows: 4.84%, 4.96%, 5.02%, 5.03%, 5.08%, it was found that the degree of crosslinking obtained by DSC measurement was higher than that obtained by xylene extraction. In the present embodiment, the formula (G) can be expressed by7-G6)/G7Error calculation for 100% to obtain five test sample passesThe errors of the cross-linking degrees obtained by the two test methods are respectively as follows: 5.81%, 5.80%, 5.81%, from which the degree of crosslinking G can be found6Degree of crosslinking G7The error between the two is about 5.8 percent, so that a correction relation G can be obtained6＝(1-5.8％)×G7. In this embodiment, the finally obtained correction relational expression is a linear relation, the calculation process is simple and convenient, the crosslinking degree obtained by the operator through the DSC test can be directly converted into the crosslinking degree of the xylene extraction test, and the requirement can be met without a complicated conversion process.
In conclusion, if the extraction time is short, the EVA and POE adhesive film samples can not be completely extracted, so that the measured crosslinking degree has errors, and meanwhile, the time required by complete extraction cannot be met in industrial production, and the production efficiency is too low. The time required by the DSC test method is only 20-30 minutes, so that the test time is greatly saved, but the DSC test has errors in the size of the crosslinking degree due to the influence of the sampling position and the laminating temperature. Therefore, the sample is subjected to the vulcanization test before the DSC test, the vulcanization test area is small, the vulcanization temperature is uniform, and the test error caused by the nonuniform lamination temperature to the DSC test can be reduced. And the sample amount required by the vulcanization test and the DSC test is small, the test time is short, and the test efficiency is greatly improved. Meanwhile, the usage amount of the adhesive film during the detection of the crosslinking degree can be saved, thereby reducing the waste of the adhesive film. The method also comprises the step of comparing and analyzing the crosslinking degree obtained by the xylene extraction method with the crosslinking degree obtained by performing DSC test after the sample is vulcanized to obtain a relational expression between the crosslinking degree obtained by the xylene extraction method and the crosslinking degree obtained by the DSC test, so that the test result of the xylene extraction method is corrected, and the crosslinking degree of the xylene extraction method can be obtained through conversion of the DSC test result. At present, a plurality of manufacturers still adopt a xylene extraction method to test the crosslinking degree, and the method can convert the DSC testing crosslinking degree into the crosslinking degree of the xylene extraction method by correcting a relational expression, so that the manufacturers can accept the testing result more easily. The method combines the vulcanization test and the DSC test, so that the influence of the lamination temperature on the DSC test result can be improved, the test efficiency can be improved, the waste of the adhesive film and the test error of the chemical-xylene extraction method can be reduced, and the reliability of the test result can be improved.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (9)
1. A method of correcting cross-linking degree test errors, comprising the steps of:
s11: sampling at different positions of the same laminated adhesive film to obtain a total test sample, dividing the total test sample into a sample A and a sample B, and dividing an un-laminated adhesive film into a sample C and a sample D;
s12: respectively preparing the sample A, the sample B, the sample C and the sample D, testing the sample A and the sample C after sample preparation by using a differential scanning calorimetry method, testing the sample B after sample preparation by using a xylene extraction method, testing the sample D after sample preparation by using a vulcanization test, and testing the sample D after the vulcanization test by using the differential scanning calorimetry method;
s13: calculating the degree of crosslinking G according to the data obtained after the sample B is completely extracted by a xylene extraction method6The sample D is subjected to a vulcanization test and then subjected to a differential scanning calorimetry test to obtain the sample DData calculation of the degree of crosslinking G7(ii) a According to the relative error calculation formula (G)7-G6)/G7X 100% calculation of the degree of crosslinking G6With the degree of crosslinking G7Relative error therebetween;
s14: repeating the calculation process of step S13 to obtain a plurality of relative errors; analyzing according to the relative errors to obtain the crosslinking degree G6With the degree of crosslinking G7The correction relation is linear relation.
2. The method of correcting errors in testing cross-linking degree of claim 1, wherein the correction relationship is: g6＝(1-5.8％)×G7。
3. The method of claim 1, wherein the total test sample is a sum of samples taken from four sides and a center of the same laminated film.
4. The method for correcting errors in testing cross-linking degree according to claim 1, wherein the sample preparation in step S12 comprises:
weighing the sample A and the sample C, wherein the total mass of each sample is in the range of 7-10 mg;
taking 460 grams of the sample B and cutting it into a number of 2mm by 2mm particles;
the sample D was cut into several 30mm by 30mm samples.
5. The method for correcting testing error of degree of crosslinking according to claim 4, wherein the differential scanning calorimetry test in step S12 comprises the steps of:
s21: opening the differential scanning calorimeter, setting parameters, adopting a program to heat up, and controlling the heating rate to be 8-12K/min;
s22: respectively placing the sample A and the sample C after sample preparation in test crucibles, uniformly contacting the bottom of each test crucible, respectively placing the two test crucibles in two furnaces, closing the furnace covers, and testing for 20-30 minutes;
s23: after the test is finished, taking out the test crucible in the furnace, and processing the differential scanning thermal curve to obtain test data;
s24: calculating the crosslinking degree G of the obtained test data according to a formula7。
6. The method for correcting testing error of crosslinking degree according to claim 5, wherein the calculation formula of crosslinking degree in step S24 is: g7＝(H1-H2)/H1X 100%, wherein, H1Denotes the heat-release enthalpy, H, of the unlaminated sample2Indicating the exothermic enthalpy of the lamination sample.
7. The method for correcting testing error of crosslinking degree according to claim 4, wherein the xylene extraction test in step S12 comprises the following steps:
s31: cleaning, drying and weighing a stainless steel wire mesh bag, wherein the weight of the mesh bag is W1Respectively putting the sample B after sample preparation into five net bags, respectively sealing the bag openings to prepare sample bags, and weighing the sample bags, wherein the weight of each sample bag is W2；
S32: putting the five sample bags into a boiling dimethylbenzene solvent for extraction, wherein the extraction time is set to be 5 hours, immediately putting the sample bags into a vacuum oven after the extraction is finished, setting the temperature of the oven to be 130 ℃, and drying for 4 hours;
s33: taking the five sample bags out of the vacuum oven, cooling and weighing, wherein the weight of the extracted sample bags is W3；
S34: the weight W obtained by the test1、W2And W3The degree of crosslinking G is calculated according to the formula6。
8. The method for correcting errors in testing cross-linking degree according to claim 7, wherein the step S34 is performed inThe cross-linking degree of (c) is calculated by the following formula: g6＝(W3-W1)/(W2-W1)×100％。
9. The method for correcting errors in a cross-linking degree test according to claim 1, wherein the parameters of the vulcanization test in the step S12 are set to be the same as the lamination parameters of the laminator.
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