Evaluation method for sealants
A four-step evaluation method assesses primer suitability for sealants in building joints, addressing delamination issues by quantitatively evaluating adhesive strength under environmental conditions, ensuring long-term waterproofing reliability.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- KAJIMA CORP
- Filing Date
- 2024-12-24
- Publication Date
- 2026-07-06
AI Technical Summary
There is no established quantitative method for selecting the optimal primer for sealants to ensure long-term reliability of waterproofing joints in exterior walls of buildings, particularly for working joints that undergo repeated compressive and tensile deformation, leading to delamination issues at the interfaces.
A four-step evaluation method involving primer application, compression and tensile deformation testing, static tensile testing, dynamic viscoelastic testing, and determining adhesive peel strength to assess the suitability of primers under actual building conditions.
Enables quantitative evaluation of primer suitability, ensuring long-term reliability of waterproofing joints by determining adhesive strength under varying environmental conditions, thereby preventing delamination.
Smart Images

Figure 2026111798000001_ABST
Abstract
Description
[Technical Field]
[0001] The present invention relates to a method for evaluating sealing materials. [Background technology]
[0002] Building sealants are used to fill the joints in the exterior walls of buildings (the joints between exterior wall members) to ensure waterproofing. The waterproofing performance of joint waterproofing, which involves filling the joints with sealant to ensure watertightness, is greatly influenced by the performance of the sealant selected for the materials, construction method, and location of the joint. Generally, the performance of sealants is described in Non-Patent Document 1, which categorizes them by type and class, by main component, by product form, by durability, and by various other performance characteristics. The test methods are described in Non-Patent Document 2.
[0003] On the other hand, exterior wall joints to be constructed include working joints and non-working joints. The former are joints with relatively large movement (movement of the joint), while the latter are joints with small or no movement. Joint waterproofing requires the selection of the appropriate type of sealant based on the combination of sealant, construction method, location, and constituent materials, and long-term watertightness is required. In particular, for working joints, the physical properties of the sealant that can follow the movement, as well as the adhesion to the constituent material (the surface to which the sealant comes into contact, hereinafter referred to as the adherend), are important. Since sealants do not have sufficient adhesion to all adherends, a primer is applied to the adherend to ensure adhesive strength before the sealant is applied. This primer plays a role in reinforcing the adhesion between the adherend / primer and between the primer / sealant, and it is necessary to select the most suitable one for the adherend and sealant. While adhesion tests for sealants are shown in Non-Patent Literature 2, there are no quantitative criteria for judgment, and there is room for improvement.
[0004] As described above, a challenge is that there is no established method for selecting the optimal primer according to the sealant and substrate. The main text of JASS8 in Non-Patent Document 3 states that "the primer to be used should be one specified by the sealant manufacturer," and the commentary on JASS8 in Non-Patent Document 3 only states that "it is necessary to use the primer specified by the sealant manufacturer and to confirm the adhesion in advance." [Prior art documents] [Non-patent literature]
[0005] [Non-Patent Document 1] JIS A 5758:2022 "Sealants for Buildings" (Japan Standards Association) [Non-Patent Document 2] JIS A 1439:2022 "Test Methods for Building Sealants" (Japan Standards Association) [Non-Patent Document 3] JASS8 T-501-2014 Performance Evaluation Test Method for Membrane Waterproofing Layers 3.3 Fatigue Test (Standard Specifications for Building Construction and Commentary, Waterproofing Work, Architectural Institute of Japan) [Overview of the Initiative] [Problems that the invention aims to solve]
[0006] As mentioned earlier, working joint sealants undergo repeated compressive and tensile deformation, and it is known that delamination occurs at the interfaces between the adherend / primer and primer / sealant, especially during tensile deformation. The present invention seeks a quantitative method for evaluating sealants in order to select the optimal primer that can ensure the long-term reliability of waterproofing joints in the exterior walls of buildings.
[0007] This invention has been made in view of the above-mentioned problems, and aims to provide a quantitative method for evaluating sealing materials, with the objective of selecting the optimal primer that can ensure the long-term reliability of waterproofing joints in the exterior walls of buildings. [Means for solving the problem]
[0008] The inventors have discovered a quantitative method for evaluating sealing materials, aimed at selecting the optimal primer to ensure the long-term reliability of joint waterproofing, and have completed the present invention. Specifically, the present invention provides the following:
[0009] (1) A method for evaluating sealant used to fill joints in the exterior walls of a building, A first step involves applying a primer to a substrate and filling the substrate with a sealant, and then performing a movement test by repeatedly subjecting the substrate to compression and tensile deformation under different temperature conditions to evaluate the adhesion between the substrate and the primer, and the adhesion between the primer and the sealant. A second step involves determining the tensile stress as a mechanical property of the sealing material by static tensile testing for each temperature condition, and determining the complex modulus or storage modulus of the tensile deformation of the sealing material by dynamic viscoelastic testing. A third step is to determine, for each temperature condition, a relationship diagram between the tensile stress of the sealing material obtained in the second step and the complex modulus of elasticity of the tensile deformation of the sealing material, or a relationship diagram between the tensile stress of the sealing material obtained in the second step and the storage modulus of elasticity, A method for evaluating a sealing material, comprising: obtaining the adhesive peel strength of the primer from the first and second steps; and, based on the adhesive peel strength of the primer obtained from the first and second steps assuming the usage environment, determining the suitability of the primer under the usage environment assumed in an actual building, using the relationship diagram obtained in the third step for each temperature condition.
[0010] (1) According to the invention, the adhesiveness of the primer / sealing material combination to the adherend can be determined. Also, the adhesiveness assuming the usage environment of the primer / sealing material combination to the adherend can be evaluated. Further, in the conventional test method, the adhesive strength under individual test conditions could be obtained, whereas in the present invention, the adhesive peel strength of the adherend / primer or primer / sealing material is obtained, and it becomes possible to quantitatively determine the suitability of the specification from the values assuming the usage environment of the building and the movement of the members. Therefore, it is possible to perform a quantitative evaluation of the sealing material for the purpose of selecting an optimal primer that can ensure the long-term reliability of the joint waterproofing of the building exterior wall.
[0011] (2) An evaluation method for a sealing material filled in the joints of the exterior wall of a building, comprising: a first step of evaluating the adhesiveness between the adherend and the primer and the adhesiveness between the primer and the sealing material by subjecting a test body in which a primer is applied to the adherend and the sealing material is filled in the adherend to which the primer is applied to a movement test that repeats shear deformation for each temperature condition; a second step of obtaining the shear stress as the mechanical property of the sealing material by a static shear test and obtaining the complex elastic modulus or storage elastic modulus of the shear deformation of the sealing material by a dynamic viscoelasticity test for each temperature condition; a third step of obtaining a relationship diagram between the shear stress of the sealing material obtained in the second step and the complex elastic modulus of the shear deformation of the sealing material or obtaining a relationship diagram between the shear stress of the sealing material obtained in the second step and the storage elastic modulus for each temperature condition; a fourth step of obtaining the adhesive peel strength of the primer from the first step and the second step, and determining the suitability of the primer under the usage environment assumed in an actual building for each temperature condition using the relationship diagram obtained in the third step based on the adhesive peel strength of the primer assuming the usage environment obtained from the first step and the second step. An evaluation method for a sealing material having these steps.
[0012] (2) According to the invention, the adhesiveness of the primer / sealing material combination to the adherend can be determined. Also, the adhesiveness assuming the usage environment of the primer / sealing material combination to the adherend can be evaluated. Further, in the conventional test methods, while the adhesive strength under individual test conditions could be obtained, in the present invention, the adhesive peel strength of the adherend / primer or primer / sealing material is obtained, and from the values assuming the usage environment of the building and the movement of the members, it becomes possible to quantitatively determine the suitability of the specifications. Therefore, it is possible to perform a quantitative evaluation of the sealing material for the purpose of selecting an optimal primer that can ensure the long-term reliability of the joint waterproofing of the building exterior wall.
[0013] (3) The usage environment in the fourth step includes the air temperature of the weather conditions and the rate of change of the joint width caused by the usage members used on the exterior wall of the building, and is the evaluation method of the sealing material according to (1) or (2).
[0014] (3) According to the invention, in the fourth step, under the usage environment in actual conditions caused by the air temperature of the weather conditions and the usage members used on the exterior wall of the building, the suitability of the primer is determined, and for the purpose of selecting an optimal primer that can ensure the long-term reliability of the joint waterproofing of the building exterior wall, a quantitative evaluation of the sealing material can be performed.
[0015] (4) A step performed before the first step, and having a step of accelerating deterioration of the test specimen by any one or more of warm water immersion and heat curing in advance, and is the evaluation method of the sealing material according to (1) or (2).
[0016] (4) According to the invention, before executing the first step S1, by executing a step of accelerating deterioration, under conditions assuming that the primer 12 deteriorates due to aging deterioration or the sealing material 10 deteriorates and hardens, resulting in a decrease in adhesive force, an evaluation test of the sealing material 10 can be performed.
Advantages of the Invention
[0017] According to the present invention, it is possible to provide a quantitative method for evaluating sealing materials, with the aim of selecting the optimal primer that can ensure the long-term reliability of waterproofing joints in the exterior walls of buildings. [Brief explanation of the drawing]
[0018] [Figure 1] This is a flowchart showing an evaluation method for a sealing material according to one embodiment of the present invention. [Figure 2] This is a perspective view showing an example of a test specimen used in the evaluation method for sealing materials according to the present invention. [Figure 3] This diagram shows the details of the stretch and deformation test in movement testing. [Figure 4] This is a perspective view showing an example of a sealing material used in the dynamic viscoelasticity test in the second step. [Figure 5] This graph shows an example of a test cycle in the first process. [Figure 6] This graph shows the relationship between the tensile change rate and the referenced stress. [Figure 7] This graph shows the temperature dispersion of the complex modulus E* of tensile deformation in a sealing material. [Figure 8] This graph shows the relationship between the complex modulus of elasticity E* and tensile stress of a sealing material during tensile deformation. [Figure 9] This graph shows the complex modulus E* of the tensile deformation of the sealing material corresponding to the operating environment. [Figure 10] This graph shows the relationship between the complex modulus E* and tensile stress of test specimen A. [Figure 11] This graph shows the relationship between the complex modulus E* and tensile stress of specimen B. [Figure 12] This diagram shows the details of the shear deformation test in movement testing. [Modes for carrying out the invention]
[0019] Embodiments of the present invention will be described below with reference to the attached drawings. Building sealants are filled into the joints of the exterior walls of a building (the joints between exterior wall members) to ensure waterproof performance. An evaluation method for sealant 10 as one embodiment of the present invention is a quantitative evaluation method for sealant 10 that is filled into the joints of the exterior walls of a building, and aims to select a primer in a sealing method using the optimal sealant 10 that can ensure the long-term reliability of waterproofing of the joints of the exterior walls of a building. As shown in Figure 1, the evaluation method for sealant 10 has a first step S1, a second step S2, a third step S3, and a fourth step S4. The evaluation method for sealant 10 is performed in the order of the first step S1, the second step S2, the third step S3, and the fourth step S4.
[0020] (1st process S1) Step 1 S1 is a step in which the adhesion of the primer is evaluated by a movement test in which compression deformation and tensile deformation are repeatedly performed, as shown in Figure 1. In Step 1 S1, as shown in Figure 2, a test specimen 1 is prepared, and a movement test is performed using the prepared test specimen 1. In Step 1 S1, a test specimen 1 (see Figure 2), in which primer 12 is applied to a pair of adherends 11 and sealing material 10 is filled into the pair of adherends 11 with primer 12 applied, is evaluated by a movement test (see Figure 3) in which compression deformation and tensile deformation are repeatedly performed for each temperature condition, to evaluate the adhesion between the adherends 11 and the primer 12, and the adhesion between the primer 12 and the sealing material 10.
[0021] In preparing test specimen 1, as shown in Figure 2, a pair of adherends 11 are separated by a predetermined distance W (for example, 12 mm), a primer 12 is applied to the pair of adherends 11, a spacer 13 is placed between the longitudinal ends of the pair of adherends 11, and a sealant 10 is filled between the pair of adherends 11 to produce test specimen 1 with the shape shown in Figure 2. As an example, as shown in Figure 2, the longitudinal length L of the sealant 10 filled between the pair of adherends 11 is 50 mm, the thickness T is 12 mm, and the width W of the sealant 10 filled between the pair of adherends 11 is 12 mm.
[0022] The material to be adherend 11 is selected from components that are actually planned to be used in the actual building being evaluated, and can be, for example, metal, non-ferrous metal, concrete, resin, etc. Such adherends 11 also include those with a surface coating of polyester-based or fluororesin-based powder coatings, heat-curing coatings such as fluororesin-based coatings, or room-temperature drying coatings such as fluororesin-based coatings. The surface of adherend 11 does not have to be coated with paint. If the surface of adherend 11 is coated with paint, the primer 12 is applied on top of the paint applied to the surface of adherend 11.
[0023] A "movement test" is performed using the fabricated test specimen 1. In this movement test, test specimen 1 is subjected to repeated compression and expansion as shown in Figure 3 under a constant temperature environment. The movement test of the present invention is based on "JASS8 T-501-2014 Performance Evaluation Test Method for Membrane Waterproofing Layers 3.3 Fatigue Test". However, since the JASS8 test is not a test for sealing materials but evaluates the crack-following ability of coating waterproofing materials, this test is modified to evaluate sealing materials.
[0024] In movement testing, the deformation rate, temperature conditions (test temperature), and number of repetitions (test cycles) are set. For example, it would look like Table 1 below. For example, in Table 1, the deformation rates are 10%, 20%, and 30%, the temperature conditions are 25°C, 60°C, and -10°C, and the number of repetitions is 500. Steps 1 to 3 in Table 1 are performed sequentially from (1) to (9). Steps (1) to (9) constitute a series of movement tests.
[0025] [Table 1]
[0026] In this case, the temperature conditions are set with 25°C as the typical temperature, 60°C as the daytime maximum temperature, and -10°C as the nighttime minimum temperature. These temperatures are quoted from JASS8, with 60°C being the test temperature assuming the exposed surface is subjected to solar radiation, and -10°C being the test temperature required in most regions of Japan. The deformation rate, test temperature, and number of tests can be set arbitrarily and can be changed as needed within the specifications of the test equipment, but the order of the temperature conditions is such that the low temperature condition is last (in Table 1, -10°C is last).
[0027] The deformation rates should be performed in ascending order. In Table 1, in steps 1 to 3, the deformation rate starts at ±10%, and in the order of steps 1 to 3, the deformation rates are ±10%, ±20%, and ±30%. The number of steps can be greater, but considering the acceleration of the test, 2 to 4 steps are preferable. Note that although Table 1 only shows steps 1 to 3, there may be 4 or more steps. The compression and tensile deformation period of the movement test should be 1 cycle per minute. It is possible to make the cycle time longer than 1 minute, but considering the acceleration of the test, 1 cycle per minute is preferable.
[0028] In the movement test, the presence or absence of delamination between the adherend 11 and the primer 12, or between the primer 12 and the sealant 10, is checked. If delamination occurs between the adherend 11 and the primer 12, or between the primer 12 and the sealant 10, the deformation rate and test temperature are recorded.
[0029] The stage at which delamination occurred is evaluated at each stage, for example, "delamination occurred after completing step 1 (3)" or "delamination occurred after completing step 2 (5)". Furthermore, it is also recorded whether the delamination occurred between the substrate 11 and the primer 12, or between the primer 12 and the sealant 10. In the former case (delamination between the substrate 11 and the primer 12), it can be determined that the adhesion of the primer 12 to the substrate 11 is poor, and in the latter case (delamination between the primer 12 and the sealant 10), it can be determined that the adhesion of the sealant 10 to the primer 12 is poor. In the former case (delamination between the substrate 11 and the primer 12), it can be determined that a change in the primer 12 should be considered, and in the latter case (delamination between the primer 12 and the sealant 10), it can be determined that a change in the sealant 10 should be considered.
[0030] (2nd process S2) Step 2, S2, as shown in Figure 1, is a process in which the tensile stress is determined as a mechanical property of the sealant 10 by static tensile testing for each temperature condition, and the complex modulus of elasticity of the tensile deformation of the sealant 10 is determined by dynamic viscoelastic testing. When the dynamic characteristics of the tensile deformation of the sealant 10 are expressed by the complex modulus (dynamic modulus), the real part is called the storage modulus, and the imaginary part is called the loss modulus. In Step 2, S2, as shown in Figure 1, static tensile testing is performed to determine the displacement-load (SS) curve of the sealant 10, and dynamic viscoelastic testing is performed to obtain temperature dispersion data of the complex modulus of elasticity of the tensile deformation of the sealant 10. The static tensile test and the dynamic viscoelastic test will be described below.
[0031] (Static tensile test) A test specimen 1 (see Figure 2) identical to the one used in the movement test is prepared, and a static tensile test is performed on the untested sealant 10. In the static tensile test of the sealant 10, the same test specimen 1 used in the movement test is used, but with the primer 12 removed, the tensile stress of the sealant 10 itself can be determined as a mechanical property of the sealant 10. Specifically, using the same test specimen 1 as used in the movement test, as shown in Figure 4, a sample of the sealant 10 is sliced from the surface with a thickness of Ta=2mm, and this sample is prepared as a dumbbell-shaped test piece as shown in "JIS K 6251:2017 Vulcanized rubber and thermoplastic rubber - Method for determining tensile properties". The tensile strength is determined when the distance between gauge marks reaches a predetermined elongation, and the tensile stress of the sealant 10 itself can be determined as a mechanical property of the sealant 10. The thickness T of the sealant 10 used in test specimen 1, as shown in Figure 2, is 12 mm. Due to the molding of the test specimen and curing shrinkage, attempting to take a sample with a thickness of Ta = 2 mm results in approximately 5 layers. The average value of these 5 layers is used to determine the tensile stress of the sealant 10 itself. The dumbbell-shaped test specimen does not have to be taken from test specimen 1; it may also be prepared from a sheet of sealant 10.
[0032] This "static tensile test" is the tensile property test described in Non-Patent Document 2 above. The tensile testing machine used is one in which the maximum load during the test is adjustable within a range of 15% to 85% of the machine's capacity, the tensile speed can be adjusted to 5.5 mm / min ± 0.5 mm / min, the temperature inside the constant temperature chamber can be adjusted to -20°C ± 2°C, and the machine is equipped with a recorder that can continuously monitor the load and displacement to create a load-displacement curve.
[0033] The test temperature should preferably be the same as that used for the movement test, and a displacement-load (SS) curve should be calculated for approximately three test temperature intervals. Furthermore, the test does not need to be conducted until failure; for practical purposes, a history of loads up to a deformation rate of 60% of the initial joint width is sufficient. The load at any given displacement (deformation rate) is determined from the displacement-load (SS) curve, and the tensile stress (N / mm²) is calculated by dividing it by the bonding area between the test specimen 1 and the adherend 11. 2 )
[0034] (Dynamic viscoelasticity test) Dynamic viscoelasticity measurements are performed using a dynamic viscoelasticity measuring device and a known method (known method: JIS K6394:2007 Vulcanized rubber and thermoplastic rubber - Method for determining dynamic properties - General guidelines (kikakurui.com)). When dynamic viscoelasticity measurements are performed on the tensile deformation of the sealant 10, the complex modulus of elasticity of the tensile deformation of the sealant 10 itself can be determined while excluding the primer 12.
[0035] In this method, the same untested specimen 1 used in the movement test is used, and as an example, as shown in Figure 4, the sealant 10 is sliced from the surface with a thickness Ta = 2 mm to obtain five layers of sample. The thickness T of the sealant 10 used in specimen 1 used in Figure 2 is 12 mm, and due to specimen molding and curing shrinkage, obtaining a sample with a thickness of Ta = 2 mm results in approximately five layers. Note that the number of layers to slice is not limited to this.
[0036] For example, the sample size for one layer of the slicing sealant 10 can be approximately 50 mm in length and 2 mm in thickness, and although the width W is shown as 12 mm in Figure 2, it can be as small as 5 mm. Note that while the length L of the sample size for one layer is shown as 50 mm, in reality, 20-30 mm is sufficient. The complex modulus E of the five layers of sealant 10 is measured in the tensile mode of a dynamic viscoelasticity testing apparatus. * The complex modulus E of the 5 layers was measured and the average value was found. * Obtain temperature dispersion data in the range of -80°C to 100°C. Complex modulus of elasticity E* From the temperature dispersion data, the complex elastic modulus E of the test temperature in the movement test is obtained. * Regarding the dynamic viscoelasticity measurement, it is disclosed in Japanese Patent Application Laid-Open No. 2024-064636, "Sealing material deterioration diagnosis method and sealing material deterioration diagnosis device".
[0037] (Step S3) As shown in FIG. 1, in Step S3, for each temperature condition, a relational diagram between the tensile stress of the sealing material 10 obtained in Step S2 and the complex elastic modulus E of the tensile deformation of the sealing material 10 is obtained. * This is a step of obtaining a relational diagram.
[0038] In Step S3, from the tensile stress of the sealing material 10 for each test temperature obtained from the static tensile test and the dynamic viscoelasticity test and the complex elastic modulus E of the tensile deformation of the sealing material 10 at the test temperature, a relational diagram between the complex elastic modulus E * and the tensile stress is created. This relational diagram can also be used for the movement tests of different primers 12 with the same sealing material 10. Here, since the physical property values of the sealing material 10 are associated with the relational diagram between the complex elastic modulus E * and the tensile stress, the change of the adherend body 11 has no influence. * and the tensile stress, the change of the adherend body 11 has no influence.
[0039] (Step S4) As shown in FIG. 1, in Step S4, based on the results of Steps S1 to S3, the suitability of the primer 12 is determined. Specifically, in Step S4, the adhesive peel strength of the primer 12 (the adhesive peel strength between the adherend body 11 / primer 12 and the adhesive peel strength between the primer 12 / sealing material 10) is obtained from Steps S1 and S2, and based on the adhesive peel strength of the primer 12 assuming the use environment obtained from Steps S1 and S2, for each temperature condition, using the relational diagram obtained in Step S3, the suitability of the primer 12 under the assumed use environment in an actual building is determined.
[0040] In the fourth step S4, the "operating environment" includes the temperature (minimum temperature) of the weather conditions and the deformation rate of the joint width caused by the materials used for the exterior walls of the building. The deformation rate of the joint width indicates the change in the joint width between materials caused by fluctuations in the temperature of the materials (the temperature difference between the highest and lowest temperatures relative to the reference temperature).
[0041] The test temperature and deformation rate at which delamination occurs between the adherend 11 / primer 12 or between primer 12 / sealant 10 are determined from the movement test. The tensile stress corresponding to the deformation rate in the movement test is then determined from the displacement-load (SS) curve at the test temperature obtained from the static tensile test. This value represents the strength at which delamination occurs between the adherend 11 / primer 12 or between primer 12 / sealant 10, or the adhesive peel strength.
[0042] Based on the minimum temperature of the actual building's operating environment and the assumed deformation rate of the joint width, the complex modulus of elasticity E of the tensile deformation of the sealant 10 corresponding to the minimum temperature is calculated from the temperature dispersion data of the sealant 10. * We calculate the complex modulus E using the assumed deformation rate. * The tensile stress is determined from the relationship between the pressure and the tensile stress. This tensile stress is compared with the adhesive peel strength obtained by the test to determine the suitability of the primer 12. If the tensile stress is greater than the adhesive peel strength, there is a possibility of peeling; conversely, if it is smaller, it can be determined that there is no problem with adhesion. According to this evaluation method, the suitability of the selected primer 12 can be quantitatively determined based on the minimum temperature of the actual building's operating environment and the deformation rate of the assumed joint width.
[0043] Next, the evaluation method for the sealing material 10 of the above embodiment will be explained with reference to an example. In the example experiment, polyurethane-based sealants were evaluated on an aluminum alloy substrate 11 using three combinations of primers (test specimen A: silane-based, test specimen B: urethane-based 1, test specimen C: urethane-based 2). In this example, the sealant 10 was polyurethane-based, and the substrate 11 was also an aluminum alloy. Only the type of primer 12 was changed in three patterns, resulting in test specimens A to C. The verification was conducted by checking whether the primer 12 in each test specimen A, B, and C peeled off from the sealant 10 and / or substrate 11 in usage environments a, b, and c.
[0044] This experiment can be conducted, for example, to answer the question "Which primer is preferable to use?" when the sealant 10 and substrate 11 to be used have already been determined. Alternatively, it could be used during the design phase or on-site construction to verify which combination of polyurethane sealant from several companies and the manufacturer's recommended primer meets the required performance requirements. Currently, products are often specified by their proven names, but substrates vary from site to site, and primer combinations are based on the test data of individual manufacturers.
[0045] In the embodiment, in order to evaluate the sealing material 10, each step is performed in the order of the first step S1 to the fourth step S4 shown in Figure 1. First, test specimens A, B, and C are prepared in the same manner as test specimen 1 in Figure 2, and the movement test in the first step S1 is performed under the test conditions shown in Table 1 above. The history of the test cycles of temperature and displacement in the movement test is shown in Figure 5. In Figure 5, the test temperature is changed to 25°C, 60°C, and -10°C, and the displacement is increased to ±10%, ±20%, and ±30% in the order of steps 1 to 3. The results of the movement test are shown in Table 2.
[0046] [Table 2]
[0047] In the results shown in Table 2, specimen A delaminated at the stage of completing step 2 at -10°C (Table 1 (6)). Specimen B delaminated at the stage of completing step 3 at -10°C (Table 1 (9)). Specimen C did not delaminate at the stage of completing step 3 at -10°C (Table 1 (9)). At this time, the interface at which delamination occurred between the adherend 11 / primer 12 / sealant 10 should also be recorded.
[0048] Next, the physical property tests (static tensile test and dynamic viscoelasticity test) of the second step S2 are performed. From the static tensile test of the sealing material 10, the relationship between tensile deformation rate and tensile stress at each test temperature is obtained, as shown in Figure 6. From the dynamic viscoelasticity test, the complex modulus of elasticity E of the tensile deformation of the sealing material 10 is obtained, as shown in Figure 7. * Obtain a diagram of the temperature dispersion.
[0049] For example, in the case of test specimen A, delamination occurred at the stage of step 2, -10°C (Table 1 (6)), as shown in the results in Table 2. Therefore, in Figure 6, test specimen A delaminated when the tensile deformation ratio was 20% and the test temperature was -10°C, and the tensile stress in this case was 0.36 N / mm 2 Since it can be read, the peel strength of test specimen A is 0.36 N / mm 2 This can be obtained. Furthermore, in the case of test specimen B, as shown in the results in Table 2, delamination occurred at the stage of step 3, -10°C (Table 1 (9)). Therefore, in Figure 6, test specimen B delaminates when the tensile deformation ratio is 30% and the test temperature is -10°C, and the tensile stress in this case is 0.48 N / mm 2 Since it can be read, the peel strength of test specimen B is 0.48 N / mm 2 You can obtain this.
[0050] Next, using Figures 6 and 7, values corresponding to test temperatures of -10°C, 25°C, and 60°C are extracted, and in the third step S3, as shown in Figure 8, the complex modulus of elasticity E of the tensile deformation of the sealing material 10 is calculated. * A diagram showing the relationship between the tensile stress of the sealing material 10 and the tensile stress of the sealing material 10 is obtained.
[0051] Next, in the fourth step S4, the applicability of the primer 12 is examined under the usage environments a, b, and c shown in Table 3 below (three levels of environments in which the sealant 10 is used (minimum temperature, deformation rate)). The fourth step S4 is a process in which the adhesive peel strength of the primer 12 (adhesive peel strength between the adherend 11 and the primer 12, and adhesive peel strength between the primer 12 and the sealant 10) is obtained from the first step S1 and the second step S2, and based on the adhesive peel strength of the primer 12 assumed to be used in the usage environment obtained from the first step S1 and the second step S2, the suitability of the primer 12 under the usage environment assumed in the actual building is determined for each temperature condition using the relationship diagram obtained in the third step S3.
[0052] [Table 3]
[0053] Here, the complex modulus of elasticity E of the tensile deformation of the sealing material 10 is * As shown in Figure 9, the complex modulus of elasticity E of the tensile deformation of the sealing material 10 under the temperature conditions a, b, and c of the above-mentioned usage environments is due to the temperature distribution. * This will be calculated for each usage environment a, b, and c.
[0054] And the complex modulus E in Figure 8 * Based on the relationship between the peel strength of the peeled specimen A and specimen B, and the complex modulus E for each usage environment a, b, and c, the peel strength of the peeled specimen A and specimen B is determined. * Comparing these values, the graphs in Figures 10 and 11 are obtained. The graph for test specimen C is omitted here. Summarizing these results, the evaluation in Table 4 below is obtained.
[0055] [Table 4]
[0056] The evaluation results for test specimen A will now be explained. For test specimen A, the tensile stress was 0.36 N / mm², which is the peel strength of test specimen A obtained in the first step S1. 2 (See Figure 6) The determination is made based on whether it is less than or greater than the specified value.
[0057] As shown in Figure 10, the complex modulus E of test specimen A at the operating environment a (minimum temperature -15°C) * The tensile stress obtained from this value, when the deformation rate is 10%, is the peel strength of test specimen A obtained in the first step S1, which is 0.36 N / mm². 2 The following is estimated (○), and the complex modulus E in the operating environment b (minimum temperature 0 degrees) * The tensile stress obtained from the values is 0.36 N / mm² for the peel strength of test specimen A obtained in the first step S1 when the deformation ratio is 10% and 20%. 2 The following is estimated (○), and the tensile stress in the operating environment c (minimum temperature 10℃) is, when the deformation rate is 10-30%, the peel strength of test specimen A obtained in the first step S1 is 0.36 N / mm 2 The following is presumed (○): For test specimen A, the peel strength of test specimen A obtained in the first step S1 is 0.36 N / mm² when the deformation rate is 20% and 30% in usage environment a, and when the deformation rate is 30% in usage environment b. 2 It is presumed to be unsuitable because it exceeds (×). Furthermore, at this time, it can be determined from the test results obtained in the first step S1 whether delamination may occur between the adherend 11 and the primer 12, or between the primer 12 and the sealant 10.
[0058] The evaluation results for test specimen B will now be explained. For test specimen B, the tensile stress was equal to the peel strength of test specimen B obtained in the first step S1, which was 0.48 N / mm². 2 (See Figure 6) The determination is made based on whether it is less than or greater than the specified value.
[0059] As shown in Figure 11, for test specimen B, the tensile stress in the operating environment a (minimum temperature -15°C) is 0.48 N / mm² when the deformation rate is 10% and 20%. 2 The following is estimated (○), and the tensile stress in usage environments b and c is, when the deformation rate is 10-30%, the peel strength of test specimen B obtained in the first step S1 is 0.48 N / mm 2The following is estimated (○): For test specimen B, the tensile stress in usage environment a is, when the deformation rate is 30%, the peel strength of test specimen B obtained in the first step S1 is 0.48 N / mm 2 It can be presumed to be unsuitable because it exceeds (×). Furthermore, at this time, it can be determined from the test results obtained in the first step S1 whether delamination may occur between the adherend 11 and the primer 12, or between the primer 12 and the sealant 10.
[0060] Test specimen C has a complex modulus E * The tensile stress calculated from this value can be estimated to be below the peel strength (○), therefore, it can be estimated that peeling will not occur within the range of the test conditions.
[0061] By evaluating whether delamination can occur between the adherend 11 / primer 12 or between the primer 12 and the sealant 10, as described in the above examples of the evaluation method for the sealant 10, the adhesion between the adherend 11 / primer 12 or between the primer 12 and the sealant 10 can be evaluated.
[0062] Thus, the evaluation method for the sealing material 10 according to the present invention allows for the determination of the adhesion of the primer 12 / sealing material 10 combination to the adherend 11. Furthermore, it allows for the evaluation of the adhesion of the primer 12 / sealing material 10 combination to the adherend 11 under conditions of use. In addition, while conventional test methods could determine the adhesive strength under individual test conditions, the present invention allows for the determination of the adhesive peel strength of the adherend 11 / primer 12 or primer 12 / sealing material 10, enabling a quantitative determination of the suitability of the specifications based on values that assume the building's usage environment and the movement of the components.
[0063] Although embodiments of the present invention have been described above, the present invention is not limited to the embodiments described above and can be modified as appropriate.
[0064] For example, in the above embodiment, the movement test in the first step S1 is shown as an example of a movement test in which compression deformation and tensile deformation are repeated (see Figure 3), but it is not limited to this, and can be replaced with a movement test in which shear deformation is repeated as shown in Figure 12. In this case, in the first step S1 of the embodiment, a movement test involving repeated shear deformation is performed instead of a movement test involving repeated compression and tensile deformation. In the second step S2 of the embodiment, for each temperature condition, the shear stress is determined as a mechanical property of the sealing material by a static shear test, and the complex modulus of elasticity or storage modulus of elasticity of the shear deformation of the sealing material is determined by a dynamic viscoelasticity test. In the third step S3 of the embodiment, for each temperature condition, a relationship diagram is obtained between the shear stress of the sealing material obtained in the second step and the complex modulus of elasticity of the shear deformation of the sealing material. In the fourth step S4 of the embodiment, the adhesive peel strength of the primer is obtained from the first and second steps, and based on the adhesive peel strength of the primer obtained from the first and second steps assuming the usage environment, the suitability of the primer under the usage environment assumed in an actual building is determined for each temperature condition using the relationship diagram obtained in the third step. As a result, similar to the embodiment described above, the evaluation method for the sealant 10 allows for the determination of the adhesion of the primer 12 / sealant 10 combination to the adherend 11. Furthermore, the adhesion of the primer 12 / sealant 10 combination to the adherend 11 can be evaluated under conditions of use. Additionally, by determining the adhesive peel strength of the adherend 11 / primer 12 or primer 12 / sealant 10, it becomes possible to quantitatively determine the suitability of the specifications based on values that assume the building's usage environment and the movement of the components.
[0065] In the above embodiment, the complex modulus of elasticity of the tensile deformation of the sealant 10 was determined by a dynamic viscoelastic test in the second step S2, but the embodiment is not limited to this. In the second step S2, the storage modulus of elasticity of the tensile deformation of the sealant 10 may also be determined by a dynamic viscoelastic test. The storage modulus of elasticity of the sealant 10 is the real part of the complex modulus. When the storage modulus of elasticity of the sealant 10 is determined by a dynamic viscoelastic test in the second step S2, in the third step S3, a relationship diagram between the tensile stress of the sealant 10 and the storage modulus of elasticity determined in the second step S2 is obtained. Then, in the fourth step S4, based on the adhesive peel strength of the primer 12 obtained from the first step S1 and the second step S2 assuming the usage environment, the suitability of the primer 12 under the usage environment assumed in the actual building can be determined for each temperature condition using the relationship diagram obtained in the third step S3.
[0066] In the above embodiment, the movement test in the first step S1 describes an example in which an undeteriorated test specimen 1 was used for the test specimen 1 shown in Figure 2. On the other hand, due to aging, the primer 12 may deteriorate, or the sealant 10 may deteriorate and harden, causing a decrease in adhesive strength. Therefore, the test specimen 1 to be used in the evaluation method of the sealant 10 may be subjected to a step to accelerate deterioration before the first step S1, by performing one or more accelerated weathering tests, either hot water immersion or heat curing, and then the movement test may be performed. By performing a step to accelerate deterioration before executing the first step S1, the evaluation test of the sealant 10 can be performed under conditions that assume that the primer 12 will deteriorate due to aging, or that the sealant 10 will deteriorate and harden, causing a decrease in adhesive strength. [Explanation of symbols]
[0067] 1 Test specimen 10. Sealant 11 Adherent 12 Primers
Claims
1. A method for evaluating sealant used to fill joints in the exterior walls of a building, A first step involves applying a primer to a substrate and filling the substrate with a sealant, and then performing a movement test by repeatedly applying compressive and tensile deformation to the substrate at different temperature conditions to evaluate the adhesion between the substrate and the primer, and the adhesion between the primer and the sealant. A second step involves determining the tensile stress as a mechanical property of the sealing material by static tensile testing for each temperature condition, and determining the complex modulus or storage modulus of the tensile deformation of the sealing material by dynamic viscoelastic testing. A third step is to determine, for each temperature condition, a relationship diagram between the tensile stress of the sealing material obtained in the second step and the complex modulus of elasticity of the tensile deformation of the sealing material, or a relationship diagram between the tensile stress of the sealing material obtained in the second step and the storage modulus of elasticity, A method for evaluating a sealing material, comprising: obtaining the adhesive peel strength of the primer from the first and second steps; and, based on the adhesive peel strength of the primer obtained from the first and second steps assuming the usage environment, determining the suitability of the primer under the usage environment assumed in an actual building, using the relationship diagram obtained in the third step for each temperature condition.
2. A method for evaluating sealant used to fill joints in the exterior walls of a building, A first step involves applying a primer to a substrate and filling the substrate with a sealant, and then evaluating the adhesion between the substrate and the primer, and between the primer and the sealant, by performing a movement test that repeatedly applies shear deformation to the substrate at different temperature conditions. A second step involves determining the shear stress as a mechanical property of the sealing material by static shear testing for each temperature condition, and determining the complex modulus or storage modulus of the shear deformation of the sealing material by dynamic viscoelastic testing. A third step is to determine, for each temperature condition, a relationship diagram between the shear stress of the sealing material obtained in the second step and the complex modulus of elasticity of the shear deformation of the sealing material, or a relationship diagram between the shear stress of the sealing material obtained in the second step and the storage modulus of elasticity, A method for evaluating a sealing material, comprising: obtaining the adhesive peel strength of the primer from the first and second steps; and, based on the adhesive peel strength of the primer obtained from the first and second steps assuming the usage environment, determining the suitability of the primer under the usage environment assumed in an actual building, using the relationship diagram obtained in the third step for each temperature condition.
3. The method for evaluating a sealing material according to claim 1 or 2, wherein the usage environment in the fourth step includes the temperature of weather conditions and the rate of change in joint width due to the materials used for the exterior wall of the building.
4. A method for evaluating a sealing material according to claim 1 or 2, comprising a step performed before the first step, wherein the test specimen is pre-treated by one or more of the following: immersion in hot water and heat curing.