CN114235674A - Method for testing and evaluating corrosion resistance of packaging adhesive film for photovoltaic module - Google Patents

Method for testing and evaluating corrosion resistance of packaging adhesive film for photovoltaic module Download PDF

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CN114235674A
CN114235674A CN202210014038.9A CN202210014038A CN114235674A CN 114235674 A CN114235674 A CN 114235674A CN 202210014038 A CN202210014038 A CN 202210014038A CN 114235674 A CN114235674 A CN 114235674A
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adhesive film
corrosion resistance
packaging adhesive
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testing
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朱雅芝
桑燕
侯宏兵
徐旭亮
史航
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Hangzhou First Applied Material Co Ltd
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Hangzhou First Applied Material Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E10/50—Photovoltaic [PV] energy

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Abstract

The invention provides a method for testing and evaluating corrosion resistance of a packaging adhesive film for a photovoltaic module. The method comprises the following steps: a sample preparation stage: aging the laminating piece with the packaging adhesive film to strip the packaging adhesive film in the sample after aging as an adhesive film to be detected; and (3) a testing stage: placing the adhesive film to be tested in a solvent for leaching treatment to obtain the acid content in the adhesive film to be tested, and marking the acid content as C; after the adhesive film to be tested in the sample after the aging treatment is stripped, the adhesive film to be tested needs to be leached within 30 min; the corrosion resistance of the packaging adhesive film is characterized by C, wherein the larger C represents the poorer corrosion resistance of the packaging adhesive film. Based on the method, the corrosion resistance of the adhesive film in practical application can be tested and evaluated more reliably and effectively in a short time.

Description

Method for testing and evaluating corrosion resistance of packaging adhesive film for photovoltaic module
Technical Field
The invention relates to the field of photovoltaic cells, in particular to a method for testing and evaluating corrosion resistance of a packaging adhesive film for a photovoltaic module.
Background
The packaging adhesive film plays a vital role in guaranteeing the power generation life of the assembly. In the prior art, an EVA/EP packaging adhesive film is one of the mature solar cell packaging materials at home and abroad at present, and the price of the EVA/EP packaging adhesive film is lower than that of a POE packaging adhesive film, so that the realization of the goal of low-price internet surfing in the photovoltaic industry is facilitated. After long-term aging and water vapor invasion, EVA/EP adhesive films (adhesive films containing EVA raw materials) are easy to degrade molecular chains of the EVA adhesive films and release acetic acid. Meanwhile, part of the organic auxiliary agent added in the packaging adhesive film may also be decomposed into acidic substances after aging, so that the slurry, the welding strips and the like on the surface of the battery piece are corroded, and the power generation power of the assembly is further influenced. However, in the prior art, when evaluating the corrosion resistance of the packaging adhesive film, the corrosion resistance of the adhesive film is often evaluated by performing an EL (electroluminescence) test on the aged photovoltaic module and combining the power attenuation condition of the module. On one hand, the method involves more influences on the performance of the raw material components, such as the difference of the self corrosion resistance of the cell, the difference of process parameters in the preparation process of the photovoltaic module and the like, and the performance of the packaging adhesive film cannot be evaluated; on the other hand, this evaluation process usually takes a long aging time and test time. Therefore, there is a need to provide a new method for evaluating corrosion resistance, which can effectively and reliably evaluate the corrosion resistance of the packaging adhesive film for photovoltaic module in a short time.
Disclosure of Invention
The invention mainly aims to provide a method for testing and evaluating the corrosion resistance of a packaging adhesive film for a photovoltaic module, which aims to solve the problem that the corrosion resistance of the packaging adhesive film for the photovoltaic module cannot be effectively and reliably evaluated in a short time in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for testing and evaluating corrosion resistance of an encapsulant film for a photovoltaic module, the method comprising the steps of: a sample preparation stage: aging the laminating piece with the packaging adhesive film to strip the packaging adhesive film in the sample after aging as an adhesive film to be detected; and (3) a testing stage: placing the adhesive film to be tested in a solvent for leaching treatment to obtain the acid content in the adhesive film to be tested, and marking the acid content as C; after the adhesive film to be tested in the sample after the aging treatment is stripped, the adhesive film to be tested needs to be leached within 30min to obtain a leaching solution; the corrosion resistance of the packaging adhesive film is characterized by C, wherein the larger C represents the poorer corrosion resistance of the packaging adhesive film.
Further, the packaging adhesive film is an adhesive film containing ethylene-vinyl acetate copolymer in raw materials.
Further, obtaining the content of acid in the adhesive film to be detected through ion chromatography; preferably, at least part of the leaching solution is taken as a sample solution, and the sample solution is subjected to an ion chromatography test by using a formula C ═ a1×V1/m1Calculating to obtain a C value; wherein, a1Represents a measured value of the acid content in the feed solution, V1Denotes the volume of the solvent, m1The weight of the adhesive film to be measured is shown.
Further, obtaining the content of acid in the adhesive film to be detected by a titration method; preferably, the titration method comprises: taking at least part of the leaching solution as a solution to be detected, titrating the solution to be detected by adopting alkali, and carrying out titration on the solution to be detected by using a formula C ═ MX (V)2-V3)×CM×1000/m2Calculating to obtain a C value; wherein M represents the molar mass of the base, V2Indicating the volume of the solution of the test solution consuming the base, V3Represents the volume of the base-depleted solution of the blank control, CMRepresents the molar concentration of the alkali solution, m2Representing the weight of the adhesive film to be detected; further preferably, the base is potassium hydroxide and the solution of the base is an ethanol solution of potassium hydroxide.
Further, the packaging adhesive film comprises a first adhesive film and a second adhesive film, and the laminating piece is obtained by laminating glass, the first adhesive film, the battery piece, the second adhesive film and the cover plate which are sequentially laminated; the size of the packaging adhesive film is larger than or equal to that of the glass.
Furthermore, the lamination treatment temperature is 120-160 ℃, and the treatment time is 10-30 min.
Further, the temperature in the aging treatment process is-40-150 ℃, and the humidity is 80-100% RH.
Further, when the content of acetic acid in the adhesive film to be tested is obtained through ion chromatography, the leaching treatment comprises the following steps: placing the glue film to be tested into a closed container, adding a solvent into the closed container, pressing the glue film to be tested to be below the liquid level of the closed container by using a polypropylene filter screen, and then heating the closed container in a water bath; preferably, the solvent is one or more of deionized water, distilled water, or ultrapure water.
Further, the water bath heating temperature is 25-99 ℃, and the time is 0.5-4 h; preferably the water bath is heated to a level no lower than 4/5 of the liquid level in the closed container.
Further, the weight ratio of the adhesive film to be tested to the solvent in the leaching treatment process is 1 (5-50).
Further, when the content of acetic acid in the adhesive film to be tested is obtained by a titration method, the leaching treatment comprises the following steps: placing the glue film to be detected into a container, adding a solvent into the container, and then carrying out ultrasonic treatment on the solvent, wherein the solvent is a mixed solvent of one or more of toluene, xylene or tetrahydrofuran and alcohols.
Further, the ultrasonic frequency of ultrasonic treatment is 20-40 kHZ, and the ultrasonic time is 5-60 min; the preferred ultrasonic frequency is 30-40 kHZ, and the ultrasonic time is 15-30 min.
Further, in the leaching treatment process, the volume consumption of the solvent is 30-120 mL based on the weight of each gram of the adhesive film to be tested.
Generally, after long-term aging and water vapor invasion, the packaging adhesive film is easy to degrade molecular chains of the adhesive film to release a part of acid. Meanwhile, part of the organic auxiliary agent added in the packaging adhesive film may also decompose into a part of acidic substances after aging. These acidic materials (including acid decomposed from the adhesive film itself and/or acid generated by aging decomposition of some additives, such as one or more of acetic acid, phenol, carbonic acid or silanol) can corrode slurry, solder strips and the like on the surface of the battery piece, and further affect the generated power of the module. Based on the cooperation of the steps, the invention simulates the construction and aging state of the packaging adhesive film for the actual photovoltaic module so as to effectively and reliably obtain the content (namely C) of acid generated by the packaging adhesive film in the actual application (after long-term aging and water vapor invasion). And for the first time, innovatively proposes that the corrosion resistance of the packaging adhesive film can be characterized by the content of the acid, namely the larger the C value is, the worse the corrosion resistance of the packaging adhesive film is. Based on the method, the corrosion resistance of the adhesive film in practical application can be tested and evaluated more reliably and effectively in a short time, so that the degradation resistance of the adhesive film in practical application can be reflected more truly, the accuracy of the test result is further improved, and the artificial error is smaller. Meanwhile, based on the test evaluation method, the test efficiency is higher, the operation is simpler and more convenient, and the evaluation reliability is higher.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a corrosion EL test chart of a battery plate after aging for 96 hours at 125 ℃ and 95% RH by using a packaging adhesive film W with poor corrosion resistance;
FIG. 2 shows a corrosion EL test chart of a battery plate after aging for 96 hours at 125 ℃ and 95% RH by using an encapsulation adhesive film M with medium corrosion resistance;
FIG. 3 shows a corrosion EL test chart of a battery plate after aging for 96h at 125 ℃ and 95% RH by using an encapsulation adhesive film B with better corrosion resistance;
FIG. 4 shows a corrosion EL test chart of a battery plate after aging for 192h at 125 ℃ and 95% RH by using an encapsulation adhesive film W with poor corrosion resistance;
FIG. 5 shows a corrosion EL test chart of a battery plate after aging for 192h at 125 ℃ and 95% RH by using an encapsulation adhesive film M with medium corrosion resistance;
FIG. 6 shows a corrosion EL test chart of a battery plate after aging for 192h at 125 ℃ and 95% RH by using an encapsulation adhesive film B with better corrosion resistance.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background of the invention section, the prior art has a problem that the corrosion resistance of the encapsulant film for photovoltaic module cannot be effectively and reliably evaluated in a short time. In order to solve the problem, the invention provides a method for testing and evaluating the corrosion resistance of a packaging adhesive film for a photovoltaic module, which comprises the following steps: a sample preparation stage: aging the laminating piece with the packaging adhesive film to strip the packaging adhesive film in the sample after aging as an adhesive film to be detected; and (3) a testing stage: placing the adhesive film to be tested in a solvent for leaching treatment to obtain the acid content in the adhesive film to be tested, and marking the acid content as C; after the adhesive film to be tested in the sample after the aging treatment is stripped, the adhesive film to be tested needs to be leached within 30 min; the corrosion resistance of the packaging adhesive film is characterized by C, wherein the larger C represents the poorer corrosion resistance of the packaging adhesive film.
Generally, after long-term aging and water vapor invasion, the packaging adhesive film is easy to degrade molecular chains of the adhesive film to release a part of acid. Meanwhile, part of the organic auxiliary agent added in the packaging adhesive film may also decompose into a part of acidic substances after aging. These acidic materials (including acid decomposed from the adhesive film itself and/or acid generated by aging decomposition of some additives, such as one or more of acetic acid, phenol, carbonic acid or silanol) can corrode slurry, solder strips and the like on the surface of the battery piece, and further affect the generated power of the module. Based on the cooperation of the steps, the invention simulates the construction and aging state of the packaging adhesive film for the actual photovoltaic module so as to effectively and reliably obtain the content (namely C value) of acid generated by the packaging adhesive film in the actual application (after long-term aging and water vapor invasion). And for the first time, innovatively proposes that the corrosion resistance of the packaging adhesive film can be characterized by the content of the acid, namely the larger the C value is, the worse the corrosion resistance of the packaging adhesive film is. Based on the method, the corrosion resistance of the adhesive film in practical application can be tested and evaluated more reliably and effectively in a short time, so that the degradation resistance of the adhesive film in practical application can be reflected more truly, the accuracy of the test result is further improved, and the artificial error is smaller. Meanwhile, based on the test evaluation method, the test efficiency is higher, the operation is simpler and more convenient, and the evaluation reliability is higher.
Specifically, in the subsequent practical application, a person skilled in the art can selectively extract some of the batch adhesive films produced in the factory as samples, and by the test evaluation method, the corrosion resistance of the packaging adhesive film is evaluated in advance, so that the production parameters can be fed back and adjusted, and the product quality is improved.
In an alternative embodiment of the present invention, the packaging adhesive film is an adhesive film containing ethylene-vinyl acetate copolymer in raw materials, such as an EVA adhesive film, a multi-layer co-extrusion adhesive film containing EVA.
For the packaging adhesive film containing the EVA raw material, the test of the content of acetic acid generated by self degradation after aging is an important index for evaluating the corrosion resistance of the adhesive film. In a preferred embodiment of the present invention, the present invention simulates the assembly and aging state of the actual packaging adhesive film based on the synergy of the above steps, and quantitatively obtains the content of acetic acid in the actual packaging adhesive film by performing ion chromatography on the aged packaging adhesive film. Wherein, the typical ion exchange mode is that the ions to be tested replace OH from the anion exchange resin-And temporarily and selectively retained on the stationary phase. At the same time, the retained anions are replaced by OH in the leacheate-The groups are displaced and eluted from the column. Has affinity to resin than OH-The weak anions pass through the column faster than those with a stronger affinity for the anion exchange sites, a process that determines the separation between anions in the sample. And finally, conducting conductivity detection through a suppressor and a conductivity cell. In ion chromatography test, the suppressor converts cations eluted from the column into H to reduce background conductivity+Therefore, the corrosion resistance obtained by the ion chromatography test is the sum of acetic acid and acetate in the liquid to be tested. Based on the above, the invention can more reliably and effectively evaluate the corrosion resistance (including acetic acid and acetic acid converted into acetate) of the packaging adhesive film containing the EVA raw material in practical application. Meanwhile, based on the test method, the test efficiency is higher, and the operation is simpler and more convenient. It should be additionally noted that only EVA raw material in the current adhesive film material used in the photovoltaic module of the solar cell can generate acetic acidTherefore, the content of acetic acid in the tested adhesive film is the corrosion resistance of the adhesive film due to degradation and release. The content of acetic acid can be more accurately obtained by adopting the ion chromatography, so that the corrosion resistance reliability of the adhesive film is better evaluated.
In a preferred embodiment, when the content of acetic acid in the glue film to be measured is obtained by ion chromatography, the leaching treatment comprises: shearing the adhesive film to be detected into pieces with the sizes of (2-5) mmx (2-5) mm, placing the pieces into a closed container, adding a solvent into the closed container, and pressing the adhesive film to be detected below the liquid level of the closed container by using a polypropylene filter screen; the closed vessel was then heated in a water bath. Therefore, the adhesive film to be tested can be better soaked in the solvent, the leaching treatment effect is better, more acetate ions in the adhesive film to be tested can be promoted to enter the leaching solution, the leaching rate of the acetate ions is higher, and further the test result obtained by the subsequent ion chromatography can be promoted to more truly, reliably and comprehensively reflect the actual acetate content in the adhesive film to be tested.
In order to improve the leaching rate of acetate ions and further improve the test accuracy, the temperature of water bath heating is preferably 60-99 ℃, and the time is preferably 0.5-4 h; the water bath is heated to a level not lower than 4/5 of the liquid level in the closed container.
In order to further improve the leaching rate of acetate ions and further improve the test accuracy, the weight ratio of the adhesive film to be tested to the solvent in the leaching process is preferably 1 (5-50).
In order to further improve the detection accuracy of the ion chromatography, a gradient elution mode is preferably adopted in the ion chromatography test process: the elution time is 15min, the concentration of the elution mobile phase is controlled to be 2mMol within 0.01-7 min, and the concentration of the elution mobile phase is controlled to be 40mMol within 8-15 min; more preferably, the elution mobile phase is potassium hydroxide and the test apparatus is ICS-600. In practical operation, one skilled in the art can adjust the elution time and concentration by itself to improve the detection accuracy, which is not described herein.
In another optional embodiment of the invention, the content of the acid in the adhesive film to be tested can be obtained by a titration method; taking part of the leaching solution as a solution to be detected, and titrating the solution to be detected by adopting alkaliBy the formula C ═ M × (V)2-V3)×CM×1000/m2Calculating to obtain a C value; wherein M represents the molar mass of the base, V2Indicating the volume of the solution of the test solution consuming the base, V3Represents the volume of the base-depleted solution of the blank control, CMRepresents the molar concentration of the alkali solution, m2Representing the weight of the adhesive film to be detected; the blank reference sample can be a mixed solution of xylene and ethanol, or a mixed solution of toluene and ethanol, and can be determined according to the mixed solution for actual test. Further preferably, the base is potassium hydroxide and the solution of the base is an ethanol solution of potassium hydroxide. The titration method is mainly used for H in solution+The content was measured and, in addition to the acetic acid decomposed from EVA, included acids generated by the aged decomposition of some auxiliary agents such as peroxides, silane coupling agents or ester-based crosslinking agents. The titration method may be an indicator colour titration method or a potentiometric titration method.
In a preferred embodiment, the reagents required in the titration test are as follows: absolute ethyl alcohol (analytically pure AR with the water content less than or equal to 0.2%), xylene (analytically pure AR with the water content less than or equal to 0.03%), KOH reagent (analytically pure AR with the purity greater than or equal to 90%), potassium hydrogen phthalate (analytically pure AR with the purity greater than or equal to 99.8%) and bromothymol blue reagent (acid-base indicator) are used as titration test reagents. Wherein the mixed solvent is a mixed solution of xylene and absolute ethyl alcohol, and the volume ratio of the xylene to the absolute ethyl alcohol is 2: 1. The alkali standard titration solution is KOH solution with a certain concentration, and the concentration is recommended to be 0.001 mol/L-0.01 mol/L. The water has a purity specified in GB/T6682 and is at least three-grade water. The indicator is an ethanol water solution prepared with bromothymol blue with the concentration of 0.05g/100mL, wherein the volume ratio of ethanol to water is 1: 4. This standard uses bromothymol blue solution as the titration indicator. The instrument requirements are as follows: a burette (meeting the GB/T12805 requirement, the capacity is 50mL, the precision is 0.1mL), a conical flask (the conical flask with a ground glass plug and the capacity is 250mL), a beaker (the capacity is 250mL), and a measuring cylinder (the capacity is 100mL, the precision is 1 mL). An ultrasonic instrument with ultrasonic frequency above 40 kHz. Analytical balance to an accuracy of 0.1 mg.
In the actual operation process, the photovoltaic packaging adhesive film taken out from the sample piece after lamination curing and aging is subjected to ultrasonic swelling through the organic mixed solvent, so that the free acid in the packaging adhesive film is dissolved in the mixed solvent. And titrating the dissolved free acid by an acid-base titration principle to evaluate the corrosion resistance of the adhesive film. The specific steps are as follows:
1. preparing a KOH ethanol solution: weighing a certain mass of KOH solid, dissolving the KOH solid in absolute ethyl alcohol with a certain volume, dissolving, fixing the volume, and standing for 4-6 days. The concentration of the KOH ethanol solution is recommended to be 0.001-0.01 mol/L, the specific use concentration is determined according to the estimated acid content, and the titration volume of the single KOH ethanol solution is ensured to be less than 25 mL.
2. Preparation of a potassium hydrogen phthalate aqueous solution: before use, the potassium hydrogen phthalate reagent is taken out and placed in a clean container, the container is placed in an oven with the temperature of 105-110 ℃ for drying until the weight is constant, about 0.075g of the potassium hydrogen phthalate reagent is dissolved in 50g of water (the concentration is about 0.0073mol/L), and the mass (m) of the actually weighed potassium hydrogen phthalate is recorded1) Calculating the actual concentration of the potassium hydrogen phthalate solution (c)1) The result was retained to 0.0001 mol/L. Note: the concentration of the potassium hydrogen phthalate water solution is 0.01mol/L corresponding to the concentration of the KOH ethanol solution, and the potassium hydrogen phthalate water solution with proper concentration is prepared according to different KOH ethanol solutions.
3. Preparing a sample: preparing and processing a laminated piece, namely preparing 1 piece of ultra-white embossed toughened glass with the thickness not less than 200mm multiplied by 200mm, 2 pieces of packaging adhesive film samples to be tested and 1 piece of back plate. After the materials are laminated according to the structure of the ultrawhite embossed toughened glass, the adhesive film to be tested and the back plate, the lamination is carried out according to the requirement, and the cross-linking degree of the packaging adhesive film after the lamination is more than 80%. After edging the laminate, four sides were sealed with aluminum foil tape. And (4) according to the GB/T29848-2018 standard, putting the laminate into an accelerated aging environment test box under certain conditions for aging treatment.
4. Titration sample preparation, within 12h after aging, the laminate in the test box was removed and sampled at a location at least 50mm from the edge of the laminate. The packaging adhesive film is peeled off from the glass surface, and the back sheet is removed. If the back plate is embrittled to result inThe method is used for removing the PET layer of the backboard completely; the peeled packaging adhesive film is cut into small pieces of about 5mm multiplied by 5mm, and about 1g of sample is weighed (recording the actual mass M)1) Adding into a conical flask containing mixed solution (40ml xylene +20ml ethanol), sealing with glass plug, and ultrasonic treating for 15 min. The ultrasonic power is recommended to be set to be 40kHZ, so that the organic acid in the adhesive film is fully dissolved into the mixed solution after the adhesive film is swelled. The water temperature is controlled during the ultrasound, and is recommended to be lower than 40 ℃. And after the ultrasonic treatment is finished, immersing the conical flask into cold water for cooling. Note: sampling should be done at room temperature, and the laminate cannot be heat treated; and (3) after the adhesive film is stripped from the surface of the glass, adding the adhesive film into the mixed solution within 10min for sealing and ultrasonic treatment.
5. Calibration and testing, blank control: 50mL of water is taken in an erlenmeyer flask, about 0.3g of bromothymol blue solution indicator is added dropwise, and the indicator is titrated by KOH ethanol solution after standing until the end point color (light green) is reached and the indicator is kept for 1min and does not change color. Record the actual volume consumed of KOH in ethanol solution (V)1). Aqueous potassium hydrogen phthalate solution: and (3) putting 50mL of potassium hydrogen phthalate aqueous solution into a conical flask, dropwise adding about 0.3g of bromothymol blue indicator, and titrating by using a KOH ethanol solution after standing until the end point color (light green) is consistent with that of a blank control sample and the color is not changed for 30 s. Record the actual volume consumed of KOH in ethanol solution (V)2)。
6. The concentration of the KOH solution is calculated, and the concentration of the KOH ethanol solution is calculated according to the formula (1), so that 3 significant digits are reserved.
Figure BDA0003459123910000061
In the formula:
m is the mass of potassium hydrogen phthalate, and the unit is gram (g);
V1-the volume of aqueous potassium hydrogen phthalate solution depleted in KOH ethanol solution in milliliters (mL);
V2-volume of blank depleted KOH ethanol solution in milliliters (mL);
204.22 molar mass of potassium hydrogen phthalate in grams per mole (g/mol).
7. Titration of acid value of sample to be tested, blank control: 40mL of xylene and 20mL of ethanol were mixed in a conical flask and about 0.3g of bromothymol blue indicator was added dropwise, titrated with the day's nominal concentration of KOH in ethanol, to the end point color (pale green) and left unchanged for 30 s. Record the actual volume consumed of KOH in ethanol solution (V)3). Testing a titration sample: and (3) dropwise adding about 0.3g of bromothymol blue indicator into the conical flask filled with the glue film mixed solution to be detected after ultrasonic treatment, and titrating by using a KOH ethanol solution with the same day calibration concentration until the color is in a light green state and is consistent with that of a blank comparison sample, and keeping the color unchanged for at least 30 s. Record the actual volume consumed of KOH in ethanol solution (V)4)。
8. Calculation of test acid number the acid number of the sample was calculated according to equation (2) and expressed as micrograms of potassium hydroxide consumed per gram of sample, and the results were taken as integers.
Figure BDA0003459123910000071
In the formula:
c-acid number of the sample in units of micrograms per gram (ug/g);
V3-the volume of KOH ethanol solution consumed by the sample to be tested in milliliters (mL);
V4-the blank control (xylene + ethanol mixed solvent) consumes the volume of KOH ethanol solution in milliliters (mL);
C(KOH)-the actual concentration of the KOH ethanol solution in moles per liter (mol/L);
56.1-constant, molar mass of potassium hydroxide, in grams per mole (g/mol);
M1the mass of the sample in grams (g).
9. Results are shown, the same laminate was sampled for 2 specimens and the arithmetic mean of the two results was taken as the acid number of the sample tested, with the results remaining integers. If the difference between the two results and the average value exceeds 15%, the laminate is sampled again according to the previous sampling step and titrated according to the previous titration process until the two results meet the requirements.
In order to further improve the accuracy of the titration method measurement and thus improve the evaluation reliability, in a preferred embodiment, when the titration method is used to obtain the content of acetic acid in the adhesive film to be measured, the leaching treatment comprises: placing the glue film to be detected into a container, adding a solvent into the container, and then carrying out ultrasonic treatment on the solvent, wherein the solvent is a mixed solvent of one or more of toluene, xylene or tetrahydrofuran and alcohols. The ultrasonic frequency of ultrasonic treatment is 20-40 kHZ, and the ultrasonic time is 5-60 min; the preferred ultrasonic frequency is 30-40 kHZ, and the ultrasonic time is 15-30 min. In the leaching treatment process, the volume consumption of the solvent is 30-120 mL based on the weight of each gram of the adhesive film to be tested.
In order to further more accurately simulate the structure of the actual packaging adhesive film, thereby improving the testing accuracy, in an alternative embodiment, the laminated part is obtained by laminating glass, the packaging adhesive film and the cover plate which are sequentially laminated; the size of the packaging adhesive film is larger than or equal to that of the glass; the glass preferably has a size of (20 to 35) cm x (20 to 35) cm. In another optional embodiment, the packaging adhesive film comprises a first adhesive film and a second adhesive film, and the laminating piece is obtained by laminating glass, the first adhesive film, the battery piece, the second adhesive film and the cover plate which are sequentially laminated; preferably, non-adhesive films are arranged between the glass and the first adhesive film, between the first adhesive film and the battery piece, between the battery piece and the second adhesive film, and between the second adhesive film and the back plate, wherein the non-adhesive films are preferably ETFE films; further preferably, the size of the ETFE membrane is (2-5) cm x (2-5) cm.
The lamination treatment temperature is 120-160 ℃, and the treatment time is 10-30 min. The size of the adhesive film is (20-35) cm x (20-35) cm; the back sheet is selected from back sheets commonly used in practice in photovoltaic modules, such as BEC303, an imperial co-extruded back sheet, a transparent CPC back sheet or a transparent TPC back sheet. The lamination treatment can adopt the conventional lamination technical means and conventional consumables in the field, and has no special requirements, and the person skilled in the art can select the materials according to the needs of the person in the field, and the description is omitted.
In a preferred embodiment, the laminate is chamfered to remove the film around the edges and sealed with aluminum tape to prevent edge moisture ingress and delamination of the aged sample. And placing the packaging adhesive film with the edge sealed by the aluminum adhesive tape into an aging box for aging, wherein gaps are required to be reserved among samples, and the samples cannot be laminated or stacked together. Thus, each laminated piece can be ensured to be in a consistent temperature and humidity aging environment.
In order to further and more accurately simulate the actual aging state, so that the test accuracy and reliability are improved, the temperature in the aging treatment process is-40-150 ℃, and the humidity is 80-100% RH. For example, HAST, DH, HF, TC or DHUV (GB/T29848-2018) may be mentioned. When the testing method of the present invention is adopted, the aging condition can be set according to the self-requirement, and is not described herein. In view of further improving the test aging property, HAST (note: 125 ℃, 95% RH) is further preferably used as the aging condition, and the aging time can be 95-97 h.
In a preferred embodiment, within 8h after the aging is finished, taking out an aged sample meeting the test conditions (poor appearance such as delamination and bubbles between the adhesive film and the glass, between the adhesive film and the back plate, between the adhesive film and the battery piece interface), stripping about 0.3-1 g of the adhesive film from a position within 50mm from the boundary of the sample, and scraping back plate scraps on the surface of the adhesive film.
In order to further improve the accuracy of the ion chromatography test method, after the leachate after leaching treatment is taken out, the ion chromatography test needs to be carried out on the leachate within 4 hours. In the leaching stage, after the adhesive film to be tested in the aged sample is stripped, the adhesive film to be tested needs to be leached within 30 min. Preferably, in the aging treatment stage, the laminated sample after the packaging treatment needs to be aged within 12 h. If ion chromatography testing of the leachate cannot be completed within 4 hours, the leachate sample is stored in a refrigerator at a temperature of <5 ℃ for 24 hours, taken out for arrangement testing when testing is possible, and similarly, testing is completed within 4 hours after the leachate is taken out.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
Laminating and laminating according to the structure of 23cm multiplied by 23cm glass/first packaging adhesive film (EVA adhesive film W with poor corrosion resistance)/second packaging adhesive film (EVA adhesive film W with poor corrosion resistance)/back plate (BEC303), wherein the laminating temperature is 145 ℃, and the laminating time is 16 min.
After the laminated laminating piece is cooled to room temperature, the edge of the laminating piece is chamfered to remove the adhesive film overflowing from the periphery, and the periphery of the laminating piece is sealed by using an aluminum adhesive tape, so that the delamination of the aged sample caused by the entrance of edge water vapor is avoided.
And (3) aging the laminated piece with the edge sealed by the aluminum adhesive tape in an aging box, wherein gaps are required to be reserved among samples, and the samples cannot be laminated or stacked together. The sample after aging needs to be guaranteed to be free from the bad problems of delamination, bubbles and the like. The aging condition was HAST (125C-95%) for 96 h.
And taking out the laminated piece meeting the test conditions (without the bad problems of delamination, air bubbles and the like) within 8h after the aging is finished, peeling off about 0.5g of first packaging adhesive film/second packaging adhesive film at a position within 50mm from the edge, and scraping back plate scraps on the surfaces of the adhesive films.
The peeled adhesive film was cut into pieces of about 3 mm. times.3 mm in size, and 0.5000g of a sample (to the accuracy of 0.0001g) was weighed.
Putting the cut pieces into a 20ml glass bottle, adding 10ml ultrapure water, pressing the rubber membrane below the water surface by using a polypropylene filter screen (capable of keeping self stability in water at room temperature of 90 ℃ below zero), sealing the bottle cover, and heating in a water bath, wherein the water surface of a water bath kettle is not lower than 4/5 of the water surface in the bottle. The sample preparation is completed within 30min after the adhesive film is stripped from the glass.
After 3h of water bath, the glass bottle filled with the sample is taken out and cooled for 30min at room temperature (23 +/-2 ℃), and then clear liquid is sucked out by using a clean needle tube, filtered by a filter head smaller than 0.22um and filled into an ion chromatography test tube to be sealed for testing.
Ion chromatography test method test: the instrument comprises the following steps: ion chromatography (currently used is ICS-600); gradient elution method, KOH concentration is 2mMol within 0.01-7 min, and KOH concentration is 40mMol within 8-15 min.
By the formula C ═ a × V1/m1Calculation gave 358 for C.
Example 2
The difference from the example 1 is only that the adhesive film is an EVA packaging adhesive film M with moderate corrosion resistance.
By the formula C ═ a × V1/m1Calculation gave C as 245.
Example 3
The difference from the example 1 is only that the adhesive film is the EVA packaging adhesive film B with better corrosion resistance.
By the formula C ═ a × V1/m1Calculation gave 155 as C.
Example 4
The only difference from example 1 is that: and laminating the laminated piece according to a structure of 23cm multiplied by 23cm of glass/first packaging adhesive film/battery piece/second packaging adhesive film back plate (BEC303), wherein the sampling position is the independent second packaging adhesive film, the laminating temperature is 145 ℃, and the laminating time is 16 min.
By the formula C ═ a × V1/m1C was calculated to be 388.
Example 5
The only difference from example 1 is that: and (3) laminating the laminated piece according to a structure of 23cm multiplied by 23cm of glass/first packaging adhesive film/battery piece/second packaging adhesive film back plate (BEC303), wherein the first packaging adhesive film/second packaging adhesive film at the position of the battery-free piece at the edge of the assembly is sampled, the laminating temperature is 145 ℃, and the laminating time is 16 min.
By the formula C ═ a × V1/m1C was calculated to be 345.
Example 6
1. Preparing a KOH ethanol solution: weighing a certain mass of KOH solid, dissolving the KOH solid in absolute ethyl alcohol with a certain volume, dissolving, fixing the volume, and standing for 4-6 days. The concentration of the KOH ethanol solution is recommended to be 0.001-0.01 mol/L, the specific use concentration is determined according to the estimated acid content, and the titration volume of the single KOH ethanol solution is ensured to be less than 25 mL.
2. Preparation of a potassium hydrogen phthalate aqueous solution: before use, the potassium hydrogen phthalate reagent is taken out and placed in a clean container, the container is placed in an oven with the temperature of 105-110 ℃ for drying until the weight is constant, about 0.075g of the potassium hydrogen phthalate reagent is dissolved in 50g of water (the concentration is about 0.0073mol/L), and the mass (m) of the actually weighed potassium hydrogen phthalate is recorded1) Calculating the actual concentration of the potassium hydrogen phthalate solution (c)1) The result was retained to 0.0001 mol/L. Note: the concentration of the potassium hydrogen phthalate water solution is 0.01mol/L corresponding to the concentration of the KOH ethanol solution, and the potassium hydrogen phthalate water solution with proper concentration is prepared according to different KOH ethanol solutions.
3. Preparing a sample: preparing and processing a laminated piece, namely preparing 1 piece of ultra-white embossed toughened glass with the thickness not less than 200mm multiplied by 200mm, 2 pieces of packaging adhesive film samples to be tested and 1 piece of back plate. After the materials are laminated according to the structure of ultra-white embossed toughened glass/EVA film W with poor corrosion resistance/EVA film W/back plate with poor corrosion resistance, lamination is carried out according to requirements, and the cross-linking degree of the packaging film after lamination is more than 80%. After edging the laminate, four sides were sealed with aluminum foil tape. And (3) according to the GB/T29848-2018 standard, putting the laminated part into an accelerated aging environment test box under certain conditions for aging treatment.
4. Titration sample preparation, within 12h after aging, the laminate in the test box was removed and sampled at a location at least 50mm from the edge of the laminate. The packaging adhesive film is peeled off from the glass surface, and the back sheet is removed. If the backboard is embrittled and cannot be removed cleanly, at least the PET layer of the backboard needs to be completely removed; the peeled packaging adhesive film is cut into small pieces of about 5mm multiplied by 5mm, and about 1g of sample is weighed (recording the actual mass M)1) Adding into a conical flask containing mixed solution (40ml xylene +20ml ethanol), sealing with glass plug, and ultrasonic treating for 15 min. The ultrasonic power is recommended to be set to be 40kHZ, so that the organic acid in the adhesive film is fully dissolved into the mixed solution after the adhesive film is swelled. The water temperature is controlled during the ultrasound, and is recommended to be lower than 40 ℃. After the ultrasonic treatment is finished, the conical flask is immersed in cold water for coolingAnd (5) cooling. Note: sampling should be done at room temperature, and the laminate cannot be heat treated; and (3) after the adhesive film is stripped from the surface of the glass, adding the adhesive film into the mixed solution within 10min for sealing and ultrasonic treatment.
5. Calibration and testing, blank control: 50mL of water is taken in an erlenmeyer flask, about 0.3g of bromothymol blue solution indicator is added dropwise, and the indicator is titrated by KOH ethanol solution after standing until the end point color (light green) is reached and the indicator is kept for 1min and does not change color. Record the actual volume consumed of KOH in ethanol solution (V)1). Aqueous potassium hydrogen phthalate solution: and (3) putting 50mL of potassium hydrogen phthalate aqueous solution into a conical flask, dropwise adding about 0.3g of bromothymol blue indicator, and titrating by using a KOH ethanol solution after standing until the end point color (light green) is consistent with that of a blank control sample and the color is not changed for 30 s. Record the actual volume consumed of KOH in ethanol solution (V)2)。
6. The concentration of the KOH solution is calculated, and the concentration of the KOH ethanol solution is calculated according to the formula (1), so that 3 significant digits are reserved.
Figure BDA0003459123910000101
In the formula:
m is the mass of potassium hydrogen phthalate, and the unit is gram (g);
V1-the volume of aqueous potassium hydrogen phthalate solution depleted in KOH ethanol solution in milliliters (mL);
V2-volume of blank depleted KOH ethanol solution in milliliters (mL);
204.22 molar mass of potassium hydrogen phthalate in grams per mole (g/mol).
7. Titration of acid value of sample to be tested, blank control: 40mL of xylene and 20mL of ethanol were mixed in a conical flask and about 0.3g of bromothymol blue indicator was added dropwise, titrated with the day's nominal concentration of KOH in ethanol, to the end point color (pale green) and left unchanged for 30 s. Record the actual volume consumed of KOH in ethanol solution (V)3). Testing a titration sample: the ultrasonic treatment is followed by the filling of the glue to be measuredAn erlenmeyer flask of the membrane mixture solution was added drop wise with about 0.3g of bromothymol blue indicator and titrated using the day's nominal concentration of KOH ethanol solution to the end point color (pale green) and consistent with the blank control and remained non-discoloring for at least 30 seconds. Record the actual volume consumed of KOH in ethanol solution (V)4)。
8. Calculation of test acid number the acid number of the sample was calculated according to equation (2) and expressed as micrograms of potassium hydroxide consumed per gram of sample, and the results were taken as integers.
Figure BDA0003459123910000111
In the formula:
c-acid number of the sample in units of micrograms per gram (ug/g);
V3-the volume of KOH ethanol solution consumed by the sample to be tested in milliliters (mL);
V4-the blank control (xylene + ethanol mixed solvent) consumes the volume of KOH ethanol solution in milliliters (mL);
C(KOH)-the actual concentration of the KOH ethanol solution in moles per liter (mol/L);
56.1-constant, molar mass of potassium hydroxide, in grams per mole (g/mol);
M1the mass of the sample in grams (g).
9. Results are shown, the same laminate was sampled for 2 specimens and the arithmetic mean of the two results was taken as the acid number of the sample tested, with the results remaining integers. If the difference between the two results and the average value exceeds 15%, the laminate is sampled again according to the previous sampling step and titrated according to the previous titration process until the two results meet the requirements.
C is 682.
Example 7
The only difference from example 6 is that: the glue film to be tested is an EVA packaging glue film M with medium corrosion resistance, and the C value is 478.
Example 8
The only difference from example 6 is that: the glue film to be tested is an EVA packaging glue film B with better corrosion resistance, and the C value is 183.
And (3) performance characterization:
the EVA film W with poor corrosion resistance in example 1, the packaging film M with medium corrosion resistance in example 2 and the packaging film B with excellent corrosion resistance in example 3 were respectively taken, and the laminating piece was laminated according to the structure of 23cm × 23cm of glass/film/battery piece/film/back plate (BEC303), wherein the laminating temperature was 145 ℃ and the laminating time was 16 min. After being packaged, the solar photovoltaic module is subjected to EL (solar module EL defect tester) and power (solar photovoltaic module power tester) tests, and the power attenuation result is shown in Table 1.
TABLE 1
Figure BDA0003459123910000121
Note: the negative sign of the power decay result indicates the decay.
FIG. 1 shows the corrosion EL result of a battery piece after aging of a packaging adhesive film W with poor corrosion resistance for 96h at 125-95% RH. FIG. 2 shows the corrosion EL result of a battery plate after aging of a packaging adhesive film M with medium corrosion resistance for 96h at 125-95% RH. FIG. 3 shows the EL corrosion result of the battery plate after aging of the packaging adhesive film B with better corrosion resistance for 96h at 125-95% RH.
FIG. 4 shows the EL corrosion result of the cell sheet after aging of the packaging adhesive film W with poor corrosion resistance for 192h at 125-95% RH. FIG. 5 shows the corrosion EL result of the battery piece after aging of the packaging adhesive film M with medium corrosion resistance for 192h at 125-95% RH. FIG. 6 shows the EL corrosion result of the battery plate after the packaging adhesive film B with better corrosion resistance is aged for 192h at 125-95% RH.
As can be seen from examples 1, 2 and 3, it is known that the corrosion resistance of the encapsulating adhesive film of example 1 < the corrosion resistance of the encapsulating adhesive film of example 2 < the corrosion resistance of the encapsulating adhesive film of example 3 (as can be confirmed by the EL diagrams of fig. 1 to 6 and the power attenuation results of table 1). Accordingly, the value of C in example 1 > the value of C in example 2 > the value of C in example 3; as can be seen from examples 6, 7 and 8, the corrosion resistance of the encapsulating adhesive film of example 6 < the corrosion resistance of the encapsulating adhesive film of example 7 < the corrosion resistance of the encapsulating adhesive film of example 8, and accordingly, the C value in example 6 > the C value in example 7 > the C value in example 8, the evaluation method of the present invention is reliable and effective.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (13)

1. A test evaluation method for corrosion resistance of a packaging adhesive film for a photovoltaic module is characterized by comprising the following steps:
a sample preparation stage: aging the laminating piece with the packaging adhesive film to strip the packaging adhesive film in the aged sample as an adhesive film to be detected;
and (3) a testing stage: placing the adhesive film to be tested in a solvent for leaching treatment to obtain the acid content in the adhesive film to be tested, and marking the acid content as C; after the adhesive film to be tested in the sample after the aging treatment is stripped, the adhesive film to be tested needs to be leached within 30 min;
and characterizing the corrosion resistance of the packaging adhesive film by using the C, wherein the larger the C is, the poorer the corrosion resistance of the packaging adhesive film is.
2. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 1, wherein the packaging adhesive film is an adhesive film comprising ethylene-vinyl acetate copolymer in raw materials.
3. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 2, wherein the content of the acid in the adhesive film to be tested is obtained by ion chromatography;
preferably, at least part of the leachate after the leaching treatment is taken as a sample solution, and the sample solution is subjected to the ion chromatography test by the formula C ═ a1×V1/m1Calculating to obtain the C value; wherein, a1A measurement value V representing the acid content of the feed liquid1Represents the volume of the solvent, m1And representing the weight of the adhesive film to be detected.
4. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as claimed in claim 1 or 2, wherein the content of the acid in the adhesive film to be tested is obtained by a titration method;
preferably, the titration method comprises: taking at least part of the leaching solution after leaching treatment as a solution to be detected, titrating the solution to be detected by adopting alkali, and carrying out titration on the solution to be detected by using a formula C ═ MX (V)2-V3)×CM×1000/m2Calculating to obtain the C value; wherein M represents the molar mass of the base, and V2Represents the volume of the solution to be measured consuming the alkali, V3Represents the volume of the solution of blank control consuming the base, CMRepresents the molar concentration of the solution of the base, m2Representing the weight of the adhesive film to be detected;
further preferably, the alkali is potassium hydroxide, and the solution of the alkali is an ethanol solution of potassium hydroxide.
5. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in any one of claims 1 to 4, wherein the packaging adhesive film comprises a first adhesive film and a second adhesive film, and the laminated member is obtained by laminating glass, the first adhesive film, a cell sheet, the second adhesive film and a cover plate which are sequentially laminated; the size of the packaging adhesive film is larger than or equal to that of the glass.
6. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 5, wherein the lamination treatment temperature is 120-160 ℃ and the treatment time is 10-30 min.
7. The method for testing and evaluating the corrosion resistance of the encapsulant film for photovoltaic modules as claimed in any one of claims 1 to 6, wherein the temperature during the aging treatment is-40 to 150 ℃ and the humidity is 80 to 100% RH.
8. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 3, wherein when the content of acetic acid in the adhesive film to be tested is obtained by the ion chromatography, the leaching treatment comprises: putting the glue film to be tested into a closed container, adding the solvent into the closed container, pressing the glue film to be tested below the liquid level of the closed container by using a polypropylene filter screen, and then heating the closed container in a water bath; preferably, the solvent is one or more of deionized water, distilled water, or ultrapure water.
9. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 8, wherein the water bath heating temperature is 25-99 ℃ and the time is 0.5-4 h; preferably the water bath is heated to a level no lower than 4/5 of the liquid level in the closed container.
10. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 8, wherein the weight ratio of the adhesive film to be tested to the solvent in the leaching process is 1 (5-50).
11. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 4, wherein when the content of acetic acid in the adhesive film to be tested is obtained by the titration method, the leaching treatment comprises: and putting the adhesive film to be detected into a container, adding the solvent into the container, and then carrying out ultrasonic treatment on the solvent, wherein the solvent is a mixed solvent of one or more of toluene, xylene or tetrahydrofuran and alcohols.
12. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 11, wherein the ultrasonic frequency of the ultrasonic treatment is 20-40 kHZ, and the ultrasonic time is 5-60 min; preferably, the ultrasonic frequency is 30-40 kHZ, and the ultrasonic time is 15-30 min.
13. The method for testing and evaluating the corrosion resistance of the packaging adhesive film for the photovoltaic module as recited in claim 11, wherein in the leaching treatment process, the volume usage amount of the solvent is 30-120 mL based on the weight of each gram of the adhesive film to be tested.
CN202210014038.9A 2022-01-06 2022-01-06 Method for testing and evaluating corrosion resistance of packaging adhesive film for photovoltaic module Pending CN114235674A (en)

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