CN111665188A - Method for testing chemical resistance of material - Google Patents
Method for testing chemical resistance of material Download PDFInfo
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- CN111665188A CN111665188A CN201910169841.8A CN201910169841A CN111665188A CN 111665188 A CN111665188 A CN 111665188A CN 201910169841 A CN201910169841 A CN 201910169841A CN 111665188 A CN111665188 A CN 111665188A
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- material sample
- impact load
- environmental stress
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Images
Classifications
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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
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/32—Investigating strength properties of solid materials by application of mechanical stress by applying repeated or pulsating forces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0001—Type of application of the stress
- G01N2203/0005—Repeated or cyclic
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0236—Other environments
- G01N2203/024—Corrosive
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
Abstract
The invention provides a method for testing chemical resistance of a material, which comprises the following steps: obtaining a material sample to be tested, wherein the material sample comprises a contact reagent surface and an impacted surface, and the contact reagent surface is opposite to the impacted surface; contacting a predetermined area of the reagent-contacting surface with an environmental stress cracking reagent for a predetermined time; and applying an impact load perpendicular to the impacted surface to a corresponding area of the impacted surface opposite to the preset area contacting with the environmental stress cracking reagent to obtain a puncture sample of the material sample after the impact load acts on the material sample, and obtaining a chemical resistance test result of the material sample according to a puncture mode of the puncture sample. The method provided by the invention reduces the use of environmental stress cracking reagents, reduces the time investment, greatly improves the testing efficiency, reduces the influence of subjective factors on the testing result, and enables the testing result to be more objective and reliable.
Description
Technical Field
The invention belongs to the field of material performance testing, and particularly relates to a device and a method for testing chemical resistance of a material.
Background
In the field of development, production and application of materials, in particular polymeric materials, testing and evaluation of the physical properties of the materials is essential.
In the field of polymers and composites thereof, especially thermoplastic resin materials such as polycarbonate materials, environmental Stress Cracking Resistance (ESC for short) of the materials is an important chemical Resistance property, which reflects the tendency of the materials to generate Stress cracks under the influence of specific chemical agents. For example, organic solvents are present in coatings, detergents or cosmetics which are in widespread contact with polycarbonates in everyday use, and these organic solvents may lead to a reduction in the mechanical properties of the polycarbonate. Many applications involving polycarbonate materials have chemical resistance as an important performance criterion. The chemical agent used in testing the environmental stress cracking performance (hereinafter referred to as environmental stress cracking agent) may be, for example, a fat, an oil, an animal fat or an organic solvent, and the like.
Current methods of testing environmental stress cracking performance in general include ISO 22088-2: 2006 (E). In the method, a material sample is first fixed; then applying a certain static load to the composite material to ensure that the composite material keeps a certain deformation; then contacting one surface of the material sample to be tested with an environmental stress cracking reagent; after a period of time (e.g., 24 hours or one week), visually inspecting the side of the material sample in contact with the environmental stress cracking agent for cracks or fissures; releasing the fixation of the material sample; and (4) performing tensile mechanical test on the material sample to obtain an environmental stress cracking performance test result. For the cracked sample of material, the time between application of the static load and cracking of the sample was recorded to evaluate the environmental stress cracking performance of the material.
US patent 4829839 discloses a method and apparatus for testing articles made from polymers such as ABS, polycarbonate, polystyrene and blends thereof for environmental stress cracking performance. The method comprises applying an environmental stress cracking agent to one side of the article, applying a static load to the other side of the article and below a horizontal plate positioned in accordance with the article, and using a timing device to record the time between application of the load and cracking of the article.
In the method for testing environmental stress cracking performance in the prior art, because the position of generating cracks, fissures or cracks on the sample workpiece is uncertain, the environmental stress cracking reagent needs to be coated on a large range of the material sample workpiece, such as the whole surface, even the material sample workpiece needs to be completely immersed in the environmental stress cracking reagent, and accordingly, a large amount of the environmental stress cracking reagent needs to be used. In prior methods, the deformation required to be applied to the material sample in advance and held in the deformed state for a period of time. In industrial production, in addition to occupying equipment for applying deformation, if the setting time is long, the production efficiency tends to be lowered, especially in the case where a large number of samples need to be continuously tested. In the existing method, the obtained environmental stress cracking performance only describes the cracks, fissures or cracking performance of the material under long-term static load, and cannot meet the test requirements of complex application environment on the material performance.
Therefore, there is a need in the art to provide a method for testing the chemical resistance of a material, which can complete the test quickly and efficiently and sufficiently reflect the environmental stress cracking performance of the material.
Disclosure of Invention
It is an object of the present invention to provide a method for testing the chemical resistance of a material. The method comprises the following steps: obtaining a material sample to be tested, wherein the material sample comprises a contact reagent surface and an impacted surface, and the contact reagent surface is opposite to the impacted surface; contacting a predetermined area of the reagent-contacting surface with an environmental stress cracking reagent for a predetermined time; and applying an impact load perpendicular to the impacted surface to a corresponding area of the impacted surface opposite to the preset area contacting with the environmental stress cracking reagent to obtain a puncture sample of the material sample after the impact load acts on the material sample, and obtaining a chemical resistance test result of the material sample according to a puncture mode of the puncture sample. Further, the method may further comprise the steps of: the impact load is applied through an impact part, the change of the impact load and the displacement of the impact part along with the time is detected in the process of applying the impact load, and the chemical resistance quantitative test result of the material sample is determined according to the change of the impact load and the displacement along with the time.
The material sample may be a material sample comprising a material prepared from one or more thermoplastic resin materials or thermosetting resin materials or a composite thereof.
The environmental stress cracking agent comprises one or more of organic solvents, coatings, paints, edible oils, beverages, skin care chemicals, cosmetics, disinfectants, and detergents.
The predetermined area of the reagent contacting face may be an area surrounding a geometric center of the reagent contacting face, such as a substantially or circular-like area centered about the geometric center, or the like.
The contacting with the environmental stress cracking agent may be by applying the environmental stress cracking agent in the predetermined area by painting, wiping, dropping, spraying, sprinkling, or the like.
The predetermined time may be determined based on the environmental stress cracking agent used, e.g., 12 hours, 24 hours, 36 hours, 72 hours, etc.
The impact load may be applied by a multi-axis impact testing apparatus and the impact member may be an impact device of the multi-axis impact testing apparatus, such as an impact head, a striker.
The impact testing of the material samples may be performed according to the instrumented multi-axial impact standard ISO 6603.2.
Depending on the puncture pattern of the punctured sample, a qualitative test result of the chemical resistance of the material sample can generally be obtained.
According to the change of the impact load and the displacement of the impact part with time and the change of the impact load and the displacement with time, an impact load-deflection curve, a maximum impact load and total load energy of the impact load and the impact of the material sample can be obtained to determine the chemical resistance test result of the material sample.
The method for testing the chemical resistance of the material provided by the invention does not need to apply an environmental stress cracking reagent on a test sample in a large area, does not need to immerse the test sample in the environmental stress cracking reagent, reduces the use of the environmental stress cracking reagent, does not need to place the material sample in test equipment to be deformed in advance, reduces the investment of the test equipment when testing a large number of material samples, does not need to carry out real-time visual observation on cracks, cracks or cracking conditions of the material sample by testing personnel in the test process, reduces the expenditure of labor cost and the influence of human subjective factors on the test result, leads the test result to be more objective and reliable, in addition, can adopt multi-axis impact test equipment which is commonly used in the field of material performance test for equipment for applying impact load to the material sample, does not need to arrange additional equipment, and then has very short impact process, therefore, the test efficiency is very high, and the material sample piece can complete the impact test step very efficiently after the environmental stress cracking agent is applied to obtain the chemical resistance test result of the material. The method for testing the chemical property of the material can obtain a qualitative test result of the chemical resistance of the material and also can obtain a quantitative test result of the chemical resistance of the material.
Drawings
The invention will be described in further detail below with reference to the drawings and examples, which are made for the purpose of illustration only and are intended to be conceptually illustrative.
FIG. 1 is a schematic illustration of a multi-axial impact testing apparatus 100 used to test a material sample 110 in a method according to the present invention.
Fig. 2.1-2.6 are schematic illustrations of six puncture pattern examples after impact of a material sample in a method of testing chemical resistance properties of a material according to the present invention.
Fig. 3.1 and 3.2 are graphs of puncture patterns of samples of the same material after impact, without and with environmental stress cracking agents applied, respectively.
Fig. 4.1 and 4.2 are graphs of puncture patterns after impact for samples of material without and with environmental stress cracking agent, respectively, applied, of another material.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications can be made by those skilled in the art after reading the teachings of the present invention, and such equivalents also fall within the scope of the appended claims. The technical terms "first" and "second" herein are used for distinguishing expression purposes only, and are not intended to indicate their order or relative importance; the technical term "connect" means to directly connect one component to another component and/or to indirectly connect another component, and means including but not limited to mechanical means, electromagnetic means, chemical means, or any combination thereof; the terms "upper", "lower", "front", "rear", "right", "left" and derivatives thereof shall be taken to correspond to the orientation in the drawings, and the invention may assume various alternative orientations, except where expressly specified otherwise. Furthermore, the present invention allows any combination or subtraction between any individual features described or implicit in the embodiments mentioned herein, yet allowing further embodiments of the invention that may not be mentioned directly herein. In addition, for simplicity of the drawings, the same or similar features may be labeled in only one or a few places in the same drawing.
The present invention provides a method for testing the chemical resistance of a material. The method comprises the following steps: obtaining a material sample to be tested, wherein the material sample comprises a contact reagent surface and an impacted surface, and the contact reagent surface is opposite to the impacted surface; contacting a predetermined area of the reagent-contacting surface with an environmental stress cracking reagent for a predetermined time; and applying an impact load perpendicular to the impacted surface to a corresponding area of the impacted surface opposite to the preset area contacting with the environmental stress cracking reagent to obtain a puncture sample of the material sample after the impact load acts on the material sample, and obtaining a chemical resistance test result of the material sample according to a puncture mode of the puncture sample. Further, the method may further comprise the steps of: the impact load is applied through an impact part, the change of the impact load and the displacement of the impact part along with the time is detected in the process of applying the impact load, and the chemical resistance quantitative test result of the material sample is determined according to the change of the impact load and the displacement along with the time.
Firstly, a material sample to be detected is obtained, wherein the material sample comprises a contact reagent surface and an impacted surface, and the contact reagent surface is opposite to the impacted surface.
The method provided by the invention can be used for testing the environmental stress cracking performance of various materials, such as thermoplastic resin materials and composites thereof, and thermosetting resin materials and composites thereof.
Examples of the thermoplastic resin material include polyolefins such as Polyethylene (PE), polypropylene (PP), and polybutylene; styrene resins such AS Polystyrene (PS), acrylonitrile butadiene styrene copolymer (ABS), and acrylonitrile styrene copolymer (AS); polyesters such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polytrimethylene terephthalate (FIT), polyethylene naphthalate (PEN), and liquid crystal polyester; polyoxymethylene (POM), Polyamide (PA), polyorganosiloxane, Polycarbonate (PC), Polymethylmethacrylate (PMMA), polyvinyl chloride (PVC), polyphenylene sulfide (PPS), polyphenylene oxide (PPO), modified PPO, thermoplastic Polyimide (PI), Polyamideimide (PAI), Polyetherimide (PEI), Polysulfone (PSU), modified PSU, Polyethersulfone (PES), Polyketone (PK), Polyetherketone (PEK), Polyetheretherketone (PEEK), Polyetherketoneketone (PEKK), Polyarylate (PAR), Polyethernitrile (PEN), thermoplastic phenolic resin, phenoxy resin; fluorine-based resins such as Polytetrafluoroethylene (PTFE), and thermoplastic elastomers such as polystyrenes, polyolefins, polyurethanes, polyesters, polyamides, polybutadienes, polyisoprenes, and fluorine-based elastomers; copolymers, modifications, and blends of two or more thereof, polymer alloys (polymeralloy), and the like, particularly polycarbonate-based resin materials and copolycarbonate resins. The composite material of the thermoplastic resin material includes a thermoplastic resin material component, other modifying components, a filler, and the like.
Examples of the thermosetting resin material include epoxy resin, cyanate resin, phenol resin, polybutadiene and styrene copolymer resin, polybenzoxazine resin, polyimide, silicon-containing resin, bismaleimide triazine resin (BT resin), and bismaleimide resin. The composite material of the thermosetting resin material comprises a thermosetting resin material component, other modification components, a filler and the like.
Modifying ingredients such as optional flame retardants, lubricants, impact modifiers, anti-drip agents, mold release agents (e.g., pentaerythritol tetrastearate), nucleating agents, stabilizers (e.g., UV/light-stabilizers, heat stabilizers, antioxidants, transesterification inhibitors, hydrolysis protectors), antistatic agents (e.g., conductive carbon black, carbon fibers, carbon nanotubes, and organic antistatic agents such as polyalkylene ethers, alkyl sulfonates, or polyamide-containing polymers), dyes, pigments, and reinforcing agents, and the like. Fillers such as glass fibers, mineral reinforcing agents, carbon fibers, and the like.
Samples of the material to be tested that are suitable for use in the test methods of the present invention can be prepared by any known processing method such as compression molding, extrusion or injection molding, among others. Typically, the dimensions of the material sample may be prepared according to the standard on which the test is based, and may be, for example, 60mm x2mm, with one 60mm x60mm side being the reagent-contacting side and the opposite side being the impacted side.
Secondly, a preset area of the reagent contacting surface is contacted with an environmental stress cracking reagent for a preset time.
Comparative testing can be performed on samples of the material that are in contact and not in contact with the environmental stress cracking agent, respectively, during testing, so that the effect of the environmental stress cracking agent on the material samples can be analyzed by comparison to assess the chemical resistance properties of the material.
The environmental stress cracking agent may include organic solvents such as ester solvents, alcohol solvents, aromatic solvents, alkane solvents, ketone solvents. The ester solvent may include ethyl acetate, etc. The alcohol solvent may include ethanol, isopropanol, and the like. The aromatic solvent may include toluene and the like. The alkane solvent may include n-hexane and the like. The ketone solvent may include acetone, butanone, and the like. The environmental stress cracking agent may also include edible oils such as olive oil, rapeseed oil, castor oil, salad oil, and the like, which are accessible in daily life.
The environmental stress cracking agent may also include various acidic or alkaline beverages or potable dairy products, such as various carbonated beverages, various colas, sodas, juices, and the like. The environmental stress cracking agent may also include various skin care chemicals, such as sunscreens, hand creams, and the like.
The environmental stress cracking agent may also include various skin-contacting chemical cosmetic products such as lipsticks, hair sprays, nail polishes, face washes, shampoos, and the like.
The environmental stress cracking agent may also include various disinfecting solutions, detergents, and the like.
The environmental stress cracking agent may also include various coatings and paints and the like.
The contacting with the environmental stress cracking agent may be by applying the environmental stress cracking agent in the predetermined area by painting, wiping, dropping, spraying, sprinkling, or the like. The material sample may be contacted with the environmental stress cracking agent by reference to the following procedure: wiping the contact reagent surface of the material sample clean to ensure no pollution; applying an appropriate amount of an environmental stress cracking agent to a central region of a reagent-contacting face of a material sample; the environmental stress cracking agent is maintained in contact with the material sample for a predetermined period of time, for example according to ISO 22088-2: 2006(E) 24 hours of recommendation. If the environmental stress cracking agent is a liquid or solvent mixture, two drops of the environmental stress cracking agent can be dropped or sprayed onto the central region of the reagent-contacting side of the material sample. If the environmental stress cracking agent is in other forms, such as an emulsion or paste, it may be applied or smeared onto the central region of the reagent-contacting surface of the material sample.
The predetermined time for contacting the environmental stress cracking agent with the material sample can also be, for example, 12 hours, 36 hours, or 72 hours, and can be determined according to the environmental stress cracking agent and the material sample to be tested.
Then, an impact load is applied perpendicular to the impacted surface at a corresponding region of the impacted surface opposite the predetermined region in contact with the environmental stress cracking agent. The material sample is ruptured upon exposure to the impact load to produce a pierced sample. And obtaining a qualitative test result of the chemical resistance of the material sample according to the puncture mode of the puncture sample.
Qualitative test results may be obtained by a puncture pattern for puncturing the sample.
Detecting changes over time in the impact load and displacement of the impact member during application of the impact load. From the changes in the impact load and displacement over time, it is possible to obtain, for example, an impact load-deflection curve of the impact load versus the impact of the material sample, and thus a maximum impact load and a total load energy, to determine the results of a quantitative chemical resistance test of the material sample.
According to the method, the qualitative test result and the quantitative test result have obvious beneficial effects compared with the chemical resistance test in the prior art.
According to the present invention, the means for applying an impact load may be a multi-axis impact testing device commonly used in the field of material property testing. Correspondingly, the impact part can be an impact device of the multi-axis impact testing device, such as an impact head and a firing pin.
Multi-axial impact testing is commonly used in the field of material property testing to test the impact resistance of materials. The impact load-deflection curve of the tested material sample can be obtained in the multi-axis impact test, wherein the maximum impact load can reflect the maximum impact load which can be borne by the tested material sample under the set test condition. The material samples tested began to crack when impacted by this maximum impact load under the set test conditions. In the impact load-deflection curve, it generally drops after the impact load reaches a maximum. If the value of the impact load is slowly decreased, the crack of the test material sample is stably propagated, and the test material exhibits toughness. If the impact load value is suddenly reduced, the crack of the tested material sample is rapidly and unstably propagated, and the tested material is shown to be brittle. The multi-axis impact test generally requires a relatively short time, for example 1-5 minutes, which also allows for very high efficiency using the method provided by the present invention.
FIG. 1 is a schematic illustration of a multi-axial impact testing apparatus 100 used to test a material sample 110 in a method according to the present invention.
As shown in fig. 1, the multi-axis impact testing apparatus 100 includes a striker 120. The striking end of striker 120 typically has a standard geometry striking surface, such as a polished hemispherical shape, which may be, for example, 10mm or 20mm diameter hemispherical. The striking surface of striker 120 remains well lubricated. Striker 120 is typically moved at a constant velocity from top to bottom, striking material sample 110 perpendicular to the impacted face of material sample 110. The impact load of striker 120 can be precisely controlled and repeated on different material samples. The impact end of striker 120 may strike the impacted face of the material sample perpendicularly to pierce the material sample 110.
As shown in FIG. 1, multi-axial impact testing apparatus 100 also includes a structure comprised of components 130 and 140 that hold and support material specimen 110. Members 130 and 140 may be, for example, ring-like structures that hold and support material sample 110 such that material sample 110 can be pierced by striker 120 at a constant velocity in a direction perpendicular to its impacted surface and ensure that striker 120 can continue to advance a safe distance after piercing material sample 110.
As shown in fig. 1, the multi-axis impact testing apparatus 100 further includes a base 150 and a rigid structure 160 for securing the entire multi-axis impact testing apparatus 100, wherein the base 150 also includes a safe distance for the striker 120 to continue to advance after piercing the material sample 110.
In the multi-axis impact test of the material sample 110, a puncture sample of the material sample 110 after being impacted is obtained, and changes of impact load and displacement of the impact component with time can be detected, for example, changes of the impact load of the striker 120 with time, changes of the vertical displacement of the striker 120 with time, changes of the impact load of the striker 120 with displacement, and changes of the displacement of the striker 120 with impact load can be detected.
After multi-axial impact testing of material sample 110, a puncture sample of material sample 110 may be obtained. The puncture samples show different puncture patterns according to the different chemical resistance properties of the material, and the chemical resistance of the material sample can be qualitatively determined according to the puncture patterns.
According to the change of the impact load and displacement of the impact member with time, for example, an impact load-deflection curve of the impact load of the striker 120 with the impact of the material sample 110, an impact load-deflection curve of the impact load of the striker 120 in the vertical displacement, and the like can be obtained, and the maximum impact load detected in the multi-axis impact test process can also be obtained. The total load energy in the multi-axis impact test process can also be calculated according to the impact load-deflection curve. The total load energy value is the energy consumed by the material sample 110 to withstand an impact when it reaches a puncture deflection, and may be determined by calculating the area encompassed by the impact load-deflection curve within the puncture deflection distance, such as by computer analysis, area measurement, or other suitable means. Puncture deflection is the deflection at which the impact load drops to half the maximum impact load.
Taking the impact load-deflection curve obtained in the process of testing chemical resistance by adopting the invention as an example, the maximum impact load can reflect the value of the maximum impact load which can be borne by the tested material under the set test condition. Material sample 110 began to crack when impacted by this maximum impact load under the set test conditions. If the impact load value is slowly decreased, the crack of the material sample 110 is stably propagated, and the tested material shows toughness. If the impact load value drops abruptly, the crack of material sample 110 rapidly and unstably propagates and the tested material appears brittle.
Fig. 2.1-2.6 are schematic illustrations of six possible puncture pattern examples of puncture samples after impact of material sample 110 obtained according to the method of testing chemical resistance properties of the present invention. The puncture pattern of the impacted puncture sample of the material sample 110 obtained in a particular experiment may not be exactly the six pattern examples shown in fig. 2.1-2.6, but may be used for reference, or other puncture patterns used for reference may be used for reference.
The central region of material sample 110 in fig. 2.1-2.6 is the region impacted and penetrated by striker 120 after application of the environmental stress cracking agent. The environmental stress cracking performance of the material samples represented by the six puncture patterns shown in fig. 2.1 to 2.6 decreased sequentially under the same test conditions, with the environmental stress cracking performance of the material sample being the best in the puncture pattern shown in fig. 2.1 and the worst in the puncture pattern shown in fig. 2.6.
The first puncture pattern is shown in fig. 2.1. The material sample 110 after impact formed a circular fracture zone 210 in its central region, with a diameter close to and slightly larger than the diameter of the impact end of the striker 120, and no cracks or fissures outside the fracture zone 210. The first puncture pattern reflects that material sample 110 is not attacked by the environmental stress cracking agent outside of the area where the environmental stress cracking agent is applied, and thus the chemical resistance of material sample 110 is good.
A second puncture pattern is shown in fig. 2.2. The material sample 110 after impact forms a circular crack zone 210 in its central region, which has a diameter close to and slightly larger than the diameter of the impact end of the striker 120, and straight cracks are generated from the crack zone 210 outward toward the edge of the material sample 110, and the straight cracks stop or maintain a straight crack-to-edge pattern before reaching the edge of the material sample 110. The straight crack may be on one side or on opposite sides of the crack region 210.
A third puncture pattern is shown in fig. 2.3. The material sample 110 after impact formed a circular fracture zone 210 in its central region, which had a diameter close to and slightly larger than the diameter of the impact end of the striker 120, and a bending crack 230 was generated outwardly from the fracture zone 210. The bend crack 230 has a bend angle less than or equal to 90 degrees and may be on one side or on opposite sides of the crack region 210.
A fourth puncture pattern is shown in fig. 2.4. The material sample 110 after impact formed a circular fracture zone 210 in its central region, with a diameter close to and slightly larger than the diameter of the impact end of the striker 120, and a bending crack 240 was generated outwardly from the fracture zone 210. The bend crack 240 has a bend angle greater than 90 degrees and may be on one side or on opposite sides of the crack region 210.
A fifth puncture pattern is shown in fig. 2.5. The material sample 110 formed a large area fracture zone 250 in its central region after impact, and there may or may not be cracks outward from the fracture zone 250. If a crack is present, the crack is not limited in shape, and may be a straight crack or a curved crack, and may or may not extend to the edge of the material sample 110. The fifth puncture pattern reflects severe erosion of material sample 110 by the environmental stress cracking agent in and around the area to which the environmental stress cracking agent is applied, and thus the chemical resistance of material sample 110 is poor.
A sixth puncture pattern is shown in fig. 2.6. The material sample 110 breaks into several fragments such as 260, 270, and 280 after impact. The sixth puncture pattern reflects that the material sample 110 is very severely attacked by the environmental stress cracking agent in the area where the environmental stress cracking agent is applied and in the surrounding area, the mechanical properties of the material are very severely affected, and thus the chemical resistance of the material sample is very poor.
The method for testing the chemical resistance of the material can be used for qualitatively and quantitatively analyzing the appearance that a material sample treated by the environmental stress cracking agent generates cracks, cracks or fractures under the impact of instantaneous impact load and objectively reflecting the chemical resistance of the material.
The methods provided by the present invention provide a way to reproducibly test the chemical resistance of a material. From a practical perspective, the method provided by the invention can be used for detecting the product performance of the material in development and production in the field of development and production manufacturing of the material so as to improve the development and production quality and efficiency in time.
In the prior art, the mechanical properties of materials, particularly thermoplastic resin materials and their composites, are evaluated by static tensile mechanical property testing for the effect of environmental stress cracking agents. The method for testing the chemical resistance of the material provided by the invention adopts completely different ideas to test and evaluate the chemical resistance of the material. Preferably, the chemical resistance of the material is tested by the multi-axial impact test method for testing the impact resistance, and the test result of the impact resistance of the material can be simultaneously obtained besides the test result of the chemical resistance, for example, in a comparative test. The method provided by the invention is particularly suitable in certain material applications, particularly applications requiring both an evaluation of the impact resistance of the material, for example, polycarbonate for cell phone housings, automotive lighting housings, medical device housings, and the like, and an evaluation of the chemical resistance of the material.
Different from the method for testing the environmental stress cracking performance in the prior art, the method for testing the chemical resistance of the material provided by the invention does not need to measure the time from the time when the material sample is contacted with the environmental stress cracking reagent to the time when the material sample fails or deforms, but only records whether the material sample reaches the set time after the material sample is contacted with the environmental stress cracking reagent, and then the impact test is carried out when the set time is reached, and the material sample is not subjected to the pre-deformation in the set time, is in a standing state and does not occupy a testing device.
The method for testing chemical resistance provided by the invention can enable a large number of material samples to be simultaneously applied with the same or different environmental stress cracking reagents, and the material samples are kept still for a preset time (for example, 24 hours), and then multi-axial impact test is continuously carried out, so that the average test time of each material sample is greatly shortened, and the development and production efficiency is improved.
Examples of the experiments
The following examples are intended to illustrate embodiments of the invention and are not intended to limit the invention in any way. Examples include comparative examples and inventive examples.
Thermoplastic resin materials used in the experimental examples: scientific polymer (China) LtdPolycarbonate material for use in the production of articles
T4006 and
2800。
preparation of the material samples used in the examples: and (5) injection molding.
The molding apparatus used in the examples was: arburg 370S 700-.
The injection molding parameters used in the examples were: the drying temperature is 120 ℃, the drying time is 3-4 hours, and the injection molding temperature is 280-320 ℃.
Example material sample preparation criteria: prepared according to ISO 6603-2 standard, the material sample size is 60mmx60mm x2 mm.
Comparative example sample: no environmental stress cracking agent was applied to any side of the material sample.
Inventive example sample: an environmental stress cracking reagent is applied to the reagent-contacting side of the material sample.
Multi-axis impact test equipment used in the experimental examples: Ceast/DAS800, available from Instron Corporation. The apparatus employs a load cell to measure the impact load applied to a material sample and an electronic sensor to measure the deflection of the measured material sample. In the test, the impact load and the deflection are synchronously measured, and a relationship graph of the impact load and the deflection is drawn.
The standards used for the multiaxial impact testing in the experimental examples were: ISO 6603-2: 2000. the parameters of the multi-axis impact test process are set according to ISO 6603-2, the mass of the firing pin is 20kg, and the impact speed is 4.4 m/s.
Environmental stress cracking agents used in the experimental examples: butyl acetate.
The experimental process comprises the following steps: two drops of butyl acetate were added dropwise to the geometric center of the reagent-contacting side of the material sample of the inventive example at a constant temperature of 73.4 ° F (23 ℃) and left for 24 hours. The material samples in the inventive example and the comparative example were subjected to a multi-axial impact test to obtain material samplesThe corresponding impact load-deflection curve of the article. Obtaining the maximum force F according to the impact load-deflection curve of the material sampleMAnd total load energy EPAnd the puncture pattern of the material sample after impact can be obtained. Above maximum force FMTotal load energy EPAnd puncture patterns are listed in table 1. Table 1 shows polycarbonate materials
T4006 and
2800 chemical resistance test results.
FIG. 3.1 and FIG. 3.2 show the same material(s) (II)
T4006) puncture pattern after impact of material samples without and with environmental stress cracking agent applied, respectively. Fig. 3.1 shows a comparative example, where no environmental stress cracking agent is applied to the material sample, the circular cracking zone formed after the impact of the material sample is relatively regular and has a diameter comparable to the diameter of the impact end of the striker 120, and where the crack propagates slightly outward. Figure 3.2 shows an example of the invention where an environmental stress cracking agent is applied to a sample of material and the resulting circular crack area is relatively regular after impact and has a diameter comparable to the diameter of the impact end of the striker 120, although there is some outward propagation of the crack in the circular crack area, but there is no significant difference from the comparison shown in figure 3.1. Therefore, the selected environmental stress cracking reagent has no obvious influence on the material, and the tested material has stronger chemical resistance.
FIG. 4.1 and FIG. 4.2 show another material (C)
2800) A puncture pattern after impact for material samples without and with environmental stress cracking agent applied, respectively. FIG. 4.1 shows a comparative example, in which no environmental stress cracking agent was applied to a sample of materialThe circular crack area formed after the material sample is impacted is more standard, and the diameter of the circular crack area is equivalent to that of the end part of the impacting device. Fig. 4.2 shows an inventive example, where an environmental stress cracking agent is applied to a material sample, and the material sample forms a circular cracking zone in the area where the environmental stress cracking agent is applied, but the diameter of the formed circular cracking zone is much larger than the diameter of the striking end of the striker of the multi-axial impact device, and a bending crack having a bending angle larger than 90 degrees propagates outward.
Comparing fig. 4.1 and 4.2, the chemical resistance of this test material was close to the puncture pattern of the material sample shown in fig. 2.5, and it was qualitatively evident that the test material was a material that was not resistant to butyl acetate.
The classification of the puncture pattern after impact for the material samples in fig. 3.1, 3.2, 4.1 and 4.2 is also given in table 1.
TABLE 1 chemical resistance Performance test results
As shown by the results in Table 1, the polycarbonate resin was obtained 24 hours after the application of butyl acetate as compared with the case where no butyl acetate was applied
The T4006 has almost no change in impact resistance, and can be quantitatively stated that the composition is not affected by butyl acetate and has relatively strong chemical resistance.
As shown by the results in Table 1, the polycarbonate resin was obtained 24 hours after the application of butyl acetate as compared with the case where no butyl acetate was applied
2800 shows a relatively large drop in impact resistance, which quantitatively indicates that the material has a relatively high resistance to butyl acetateWeak.
The examples show that the method for testing the chemical resistance of a material provided by the invention can realize the evaluation of the chemical resistance of the material, and besides qualitatively obtaining the chemical resistance of the material according to the puncture mode of the material sample, can also provide quantitative data of the change of mechanical properties after the application of the environmental stress cracking agent, so that the chemical resistance of the material can be evaluated in a quantitative manner.
Although the invention has been described in detail in the foregoing for the purpose of illustration, it is to be understood that such detail is solely for that purpose and that variations can be made therein by those skilled in the art without departing from the spirit and scope of the invention except as it may be limited by the claims.
Claims (12)
1. A method of testing chemical resistance of a material, the method comprising the steps of:
obtaining a material sample to be tested, wherein the material sample comprises a contact reagent surface and an impacted surface, and the contact reagent surface is opposite to the impacted surface;
contacting a predetermined area of the reagent-contacting surface with an environmental stress cracking reagent for a predetermined time;
applying an impact load perpendicular to the impacted surface to a corresponding region of the impacted surface opposite the predetermined region in contact with the environmental stress cracking agent to obtain a pierced sample of the material sample after the impact load is applied, and,
and obtaining the chemical resistance test result of the material sample according to the puncture mode of the puncture sample.
2. A method according to claim 1, wherein the impact load is applied by an impact member, the impact load and displacement of the impact member are detected over time during the application of the impact load, and the results of the chemical resistance quantitative test of the material sample are determined from the changes over time in the impact load and displacement.
3. The method of claim 1 or 2, wherein the material sample comprises one or more material samples prepared from a thermoplastic resin material or a thermosetting resin material.
4. The method of claim 1 or 2, wherein the material sample comprises one or more material samples prepared from a composite of a thermoplastic resin material or a thermoset resin material.
5. The method of claim 1 or 2, wherein the environmental stress cracking agent is selected from one or more of the following: organic solvents, coatings, paints, edible oils, beverages, skin care chemicals, cosmetics, disinfectants, and detergents.
6. The method of claim 1 or 2, wherein the predetermined area of the reagent-contacting surface is an area surrounding a geometric center of the reagent-contacting surface.
7. The method of claim 6, wherein said contacting with an environmental stress cracking agent comprises one or more of painting, wiping, dropping, spraying, and sprinkling said environmental stress cracking agent on said predetermined area.
8. The method of claim 1 or 2, wherein the predetermined time is 12 hours, 24 hours, 36 hours, or 72 hours.
9. The method of claim 7, wherein the predetermined time is 12 hours, 24 hours, 36 hours, or 72 hours.
10. A method as claimed in claim 1 or 2, wherein the impact load is applied by a multi-axis impact testing apparatus and the impact member is an impact device of the multi-axis impact testing apparatus.
11. The method of claim 2, wherein determining the results of the quantitative chemical resistance test of the material sample based on the changes in the impact load and the displacement over time comprises obtaining an impact load-deflection curve of the impact load versus the impact of the material sample based on the changes in the impact load and the displacement over time.
12. The method of claim 11, wherein determining the chemical resistance quantitative test result for the material sample comprises determining a maximum impact load and a total load energy from the impact load-deflection curve to determine the chemical resistance quantitative test result for the material sample.
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| CN113155822A (en) * | 2021-04-26 | 2021-07-23 | 江西矽贝克新材料有限公司 | Method for testing anti-fogging performance of organic silicon release agent |
| CN113155716A (en) * | 2021-03-02 | 2021-07-23 | 广东聚石化学股份有限公司 | Method for detecting stress cracking resistance |
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