CN100580434C - Coating for inspection of cracking in structure - Google Patents

Coating for inspection of cracking in structure Download PDF

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Publication number
CN100580434C
CN100580434C CN200480017901A CN200480017901A CN100580434C CN 100580434 C CN100580434 C CN 100580434C CN 200480017901 A CN200480017901 A CN 200480017901A CN 200480017901 A CN200480017901 A CN 200480017901A CN 100580434 C CN100580434 C CN 100580434C
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China
Prior art keywords
overlayer
capsule
micro
liquid
cracks
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CN1813184A (en
Inventor
高桥一比古
牛岛通雄
内田光彦
小野口富夫
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ThreeBond Co Ltd
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National Maritime Research Institute
ThreeBond Co Ltd
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Abstract

The present invention provides a coating for inspection of cracking in a structure, having a coating layer, in which microcapsules having a visible liquid sealed therein are dispersed, provided on a surface of structure. When the structure is cracked, the crack is transmitted to the coating layer and microcapsules of the coating layer are broken in accordance therewith. The visible liquid having outflowed from the microcapsules moves along the crack of the coating layer and reaches the surface of the coating layer, so that the cracking of the structure can be detected. At least one second coating layer not containing microcapsules is disposed on a first coating having such microcapsules dispersed therein, which second coating layer has an outermost layer being transparent and having flexibility sufficient to be free from cracking even when the first coating layer has cracked.

Description

The inspection of cracking of structure is with covering
Technical field
The inspection of cracking that the present invention relates to a kind of structure particularly relates to the inspection covering of the fatigue cracking of various structures such as boats and ships, bridge, vehicle, aircraft, work mechanism with covering.
Background technology
Structures such as boats and ships, bridge, vehicle, aircraft, Work machine, mainly constitute by metal such as iron, aluminium, magnesium or their alloy etc., if but these metallic structures are applied load repeatedly, then concentrate portion especially can chap at its stress sometimes owing to metal fatigue.Because the fatigue cracking of such structure is slowly development along with the process of time, therefore will be regularly or irregularly carry out the inspection of cracking of structure.
In such inspection of cracking, generally carry out visual examination, under special situation, implement accurate inspection by machines such as UT (Ultrasonic Testing).For example, open in the flat 4-169836 communique the spy, disclose a kind of by obtaining the distortion amplitude of fluctuation of object structure period according to the fracture of fine rule, thereby high precision precognition fatigue damage produces the method in period.In addition, open in the flat 1-180757 communique real, disclose a kind of be full of cracks and detected place formation strip-shaped conductive film at structure, connect conducting detector at its two ends, detect the strip-shaped conductive film along with the generation of be full of cracks is ruptured by conducting detector, the method for the generation by coming the early detection fatigue cracking like this.
But above-mentioned close examination method all need the mensuration machine is set, so cost is higher, in addition, because it is complicated to measure the operation of machine, therefore needs skilled problems such as operation also more.In addition, checking that narrow place or parts install under the situation in complicated place etc., be difficult to use and measure machine and can't be suitable for.
In order to solve the problem points that the inspection method of machine is measured in such use, open in the flat 10-267866 communique (prior art 1) the spy and to disclose a kind of technology, promptly form the overlayer that is dispersed with the glass capsule of having enclosed visibleization liquid by surface at structure, the be full of cracks that is produced in the structure, also produce be full of cracks in the above-mentioned overlayer, by causing the destruction of the glass capsule in the overlayer like this, as seen change liquid and flow out to tectal surface, thereby detect the be full of cracks place.
In addition, a kind of technology is disclosed in United States Patent (USP) No. 5534289 (prior art 2), promptly form the 1st overlayer that is dispersed with the micro-capsule of having enclosed visibleization liquid on the surface of structure, 2nd overlayer different with visibleization liquid color further is set thereon, when in above-mentioned structure, having produced be full of cracks, with this crevasse crack propagation to the 1 and the 2nd overlayer, be accompanied by this action, micro-capsule is destroyed, flow out and arrive the visibleization liquid on the 2nd tectal surface along be full of cracks by detecting from micro-capsule, the be full of cracks that detects above-mentioned structure produces.In addition, here as visibleization liquid, use orchil.
As seen change in the method for liquid in the use shown in prior art 1 and 2, as seen change the be full of cracks that liquid produced in the structure and be seeped into cover surface, by being looked, it recognizes having or not of confirming to chap, but exist the visibleization liquid that is exuded to cover surface to fade gradually, become gradually and can't look the problem of recognizing along with the process of time.
In addition, in prior art 2,,, the overlayer coating that is dispersed with this micro-capsule is formed on the surface of structure mainly used as visibleization liquid with orchil microencapsulations such as azo system, anthraquinone based compounds.But, using under the situation of this visibleization liquid, visibleization of the redness liquid that be full of cracks produced that is accompanied by structure is subjected to the influence of ultraviolet ray etc. and fades gradually, thereby existence becomes gradually and can't look the problem of recognizing.
Summary of the invention
The invention that the present invention finishes in order to address the above problem just, the inspection of cracking precision that needs (visibility that causes by oozing out of dyestuff), the inspection precision of the degree that be full of cracks that the size of accidents caused danger is arranged before check next time can not missed preferably, from this position, its purpose is, even provide a kind of inspection of cracking that does not use the structure that the described measurement machine of above-mentioned prior art also can check be full of cracks simply with covering, and provide a kind of can to the be full of cracks that is produced in the structure reply and the inspection of cracking of the structure of the long-time stability of the cognitive liquid guaranteeing from damaged micro-capsule, to flow out with covering.
The inspection of cracking that the 1st form of the present invention is a kind of structure is with covering, its surface at structure forms the overlayer that is dispersed with the micro-capsule of having enclosed cognitive liquid, when producing be full of cracks in this structure, this be full of cracks is transferred to this overlayer, micro-capsule in this overlayer is destroyed thereupon, the be full of cracks of the cognitive liquid that from this micro-capsule, flows out in overlayer, arrive cover surface, the be full of cracks that so can detect this structure produces, it is characterized in that: be dispersed with the 1st of micro-capsule at this and cover, at least 1 layer the 2nd overlayer that does not contain micro-capsule is set, simultaneously, the 2nd overlayer is transparent and have an outermost layer, and described outermost layer has that it can not produce be full of cracks yet when enough flexibilities produced be full of cracks with box lunch in the 1st overlayer.
The 2nd form of the present invention, be to use in the covering at the inspection of cracking of above-mentioned structure, this outermost elongation, more than 17 times of elongation of the layer beyond the outermost layer when being the 1st tectal elongation and the layer beyond in the 2nd overlayer, having outermost layer respectively.
The 3rd form of the present invention, be to use in the covering at the inspection of cracking of above-mentioned structure, the cognitive liquid of being enclosed in this micro-capsule is a principal ingredient with nigrosine based compound and solvent, and its weight rate is the nigrosine based compound: solvent=1: 55~1: 0.37.
Description of drawings
Fig. 1 is the vertical view of employed test film in the test of fatigue cracking progress.
Fig. 2 is the side view of the test film that uses in physical property test.
Embodiment
With the 1st overlayer that covers, can use the known in the past micro-capsule overlayer that contains as the inspection of cracking that constitutes structure of the present invention basically.In this case, as the cognitive liquid that is enclosed in the micro-capsule, can use the liquid material of known in the past dyestuff or pigment dissolved and even dispersion.With regard to its object lesson, dyestuff can list dyestuffs such as azo system, anthraquinone system.In addition, these dyestuffs preferably to be dissolved in aqueous in the hydrophobic solvents such as known in the past for example mineral oil, olein acid, linoleic acid, carry out microencapsulation.
About the mixing ratio of dyestuff and solvent, not special regulation, but, preferably use dyestuff from the concentration of color, the viewpoint of solubleness: the mixing ratio of solvent=0.5: 9.5~2.5: 7.5 (weight ratio) degree.In addition, if also use as cognitive liquid, for example under the situation in the dark surrounds that structure is structured in the boats and ships, by irradiation black light with fluorescent dye, the fluorescent dye that flows out from overlayer because of be full of cracks can appear in one's mind out brightly, makes the affirmation of be full of cracks be more prone to.
The inventor etc. also study the cognitive liquid of bringing into play effect of the present invention to greatest extent, found that with nigrosine based compound and solvent be principal ingredient, its weight rate is the nigrosine based compound: solvent=1: 55~1: 0.37 has demonstrated significant more effect.The nigrosine based compound is the derivant of nigrosine or nigrosine, as its object lesson, can list solvent black (Solvent Black) 5, solvent black 7 etc., is not limited in these certainly.In addition, also be not dissolved in moisture this point such as rainwater, seawater, preferred aforesaid hydrophobic solvent when the be full of cracks color development from this case solvent.
In the blending ratio of nigrosine based compound and solvent, surpassing 55 weight portions at relative nigrosine based compound 1 weight portion cooperates under the situation of solvent, visibility is not enough, in addition, if amount of solvent less than 0.37 weight portion, then the viscosity of cognitive liquid increases, become and be difficult to microencapsulation, simultaneously, even under by the situation of microencapsulation, the visibility liquid measure that arrives the surface along be full of cracks reduces.
The 1st tectal thickness is had no particular limits, and optimum range is different because of the particle diameter of micro-capsule, but in general is 50~500 μ m, preferred especially 100~350 μ m.If less than 50 μ m, just necessary use mean grain size is than its little micro-capsule, and so, the absolute magnitude of the cognitive liquid in the capsule can be not enough, and it is very difficult destroyed that capsule becomes, and color emissivity worsens easily.In addition, if surpass 500 μ m, the be full of cracks that is produced in the structure just is difficult to propagate into the 1st tectal filming.
Particle diameter to the micro-capsule that uses among the present invention also has no particular limits, but the micro-capsule that preferably has the mean grain size of 30~300 μ m, the micro-capsule that especially preferably has the mean grain size of 50~200 μ m.If less than 30 μ m, the absolute magnitude of the cognitive liquid in the capsule can be not enough, and it is very difficult destroyed that capsule becomes, and color emissivity worsens easily.In addition, if surpass 500 μ m, the be full of cracks that is produced in the structure just is difficult to propagate into the 1st tectal filming.
In the present invention, disperse to contain the micro-capsule of cognitive liquid, thereby form the 1st overlayer, but, can preferably use employed various hardenings or curable flow-like resin combination in coating or coating agent etc. as forming this tectal material.As these resin combinations, for example can use the coating of epoxy system, carbamate system, acrylic acid series, nitrocotton system, silicone-based, modified silicone system, coating agent, coverture etc.Epoxy resin such as preferred especially bisphenol A-type or Bisphenol F type.These coating, coating agent, coverture can be principal ingredient with the reactive resin compositions that hardens by variety of ways such as heating, moisture, illumination, two liquid (two-liquid) mixing; Also can under the form of above-mentioned various resin dissolves in solvent, be coated on the bur, solidify by the evaporation of solvent; Perhaps also with these two methods.
In addition, for the micro-capsule that will contain cognitive liquid or the surface color that becomes the structure of bur stash, and in order to ensure by the caused visibility of the outflow of cognitive liquid, it is preferably opaque to form the 1st tectal bonding agent, especially preferably is colored as white color system such as white, milky.As so painted in effective material, for example can use white color system pigment or white color system filling agents such as titanium dioxide, carbide of calcium, talcum.
Next, as the manufacture method of the micro-capsule that contains cognitive liquid, can use in coacervation, original place (in-situ) polymerization, interfacial polymerization, the liquid known method in the past such as hardening process.Wherein, consider the stability of the microcapsule membrane when bur surface formation overlayer,, can use gelatin as material.
In addition, form the ratio that cooperates of the 1st tectal adhesive ingredients and the micro-capsule that contains cognitive liquid, depend on the intensive amount of cognitive liquid and the particle diameter of micro-capsule, but probably count near portions of resin micro-capsule=4: 1, or be suitable near counting 2.5: 1 with volume ratio with weight ratio.Along with the micro-capsule ratio is lower than the said reference value, the color development when be full of cracks produces just can be not enough, in addition, along with ratio increases, the destruction that when the coating of filming forms, can cause micro-capsule, or viscosity increased and be coated with difficulty.
In the present invention, coating the 2nd overlayer on formed like this 1st overlayer.The 2nd overlayer both can only be made of outermost layer, also can be the formation with layer more than 1 layer of separating with outermost layer (below be called " middle layer ").When the coating middle layer, the middle layer preferably is painted to opaque layer.By the existence in middle layer, improved the 1st tectal appearance characteristics, can improve the visibility when sending.Thickness to the middle layer has no particular limits, but preferred 50~500 μ m, preferred especially 100~350 μ m.If less than 50 μ m, then be difficult to fully manifest the function in middle layer, in addition,, then be difficult to propagate the be full of cracks that is produced in the structure if surpass 500 μ m.
Be painted to opaque tectal material (coating) as what form the middle layer, identical with the 1st overlayer, for example can use with epoxy resin, carbamate resins, acrylic resin, silicone resin, modified silicone resin various flow-like compositions as principal ingredient.Wherein, consider environmental pollution or operating environment, the resin combination of preferred reactive.Especially preferably with the identical resin of the employed composition of the 1st overlayer, epoxy resin is ideal.
By adopting,, can realize purpose of the present invention with the double-decker that the 2nd overlayer with the transparent outermost that does not contain micro-capsule is constituted by the 1st overlayer that is dispersed with the micro-capsule that has included cognitive liquid.So, though might not allow the 2nd overlayer be sandwich construction, be under the situation of multilayer at the 2nd overlayer, preferably with outermost layer as hyaline layer, with other middle layers as staying the layer that keeps color development in the layer because of the cognitive liquid that be full of cracks is flowed out.Under this meaning,, preferably adopt middle layer with tones such as white or milkys though above-mentioned middle layer is relevant with the kind of cognitive liquid.In addition, can also play and be used for preventing that the 1st tectal micro-capsule is by the effect from the protective seam that impact destroyed of outside such as slungshot.In addition, in the 1st overlayer that is dispersed with micro-capsule and transparent the 2nd tectal double-decker, owing to can't hide the color of cognitive liquid fully, so the more weak tendency of color contrast when having color development.
Form all or a part of transparent outermost of the 2nd overlayer, need have flexibility so that can not produce be full of cracks along with the be full of cracks of structure.The standard that this is flexible, though be subjected to the adhering influence of transparent outermost layer and other layers (1st overlayer, 2nd tectal middle layer) stacked with it, but require the extension of conduct layer (filming) bigger, preferably needing outermost elongation is more than 17 times of other tectal elongations.On the other hand, if the tectal elongation of outermost with respect to other overlayers less than about 5 times, then outermost layer produces the almost also generation be full of cracks simultaneously of be full of cracks at other layers, because cognitive liquid flows out from this be full of cracks, when in water/use in the seawater or during at the position that is used to drench with rain etc., be difficult to guarantee long-term visibility.In addition, contain the 1st overlayer of micro-capsule, preferably higher with the adhesiveness of structure matrix, and extend less.The 1st tectal extension is preferably below the 3mm, especially preferably below the 1mm.
In addition, the 2nd tectal outermost layer, and the shear bond power between the overlayer under it is preferably below the 1MPa.If bonding force is higher, on the layer under sticking to, then be subjected to easily structure and under the influence of displacement of layer, be easy to generate be full of cracks.Another face, if bonding force is lower, then and under overlayer between the space appears easily, be difficult to be subjected to the influence of displacement.In addition, as being used for forming the 2nd tectal outermost material, can be the various flow-like compositions of principal ingredient for example, suitably select to satisfy above-mentioned flexible person from Oppanol or styrene-butylene copolymer rubber equal solvent dilution type rubber coating, epoxy resin, carbamate resins, acrylic resin, silicone resin, modified silicone resin etc.
Outermost thickness is generally 10~500 μ m, preferred especially 20~200 μ m.If less than 10 μ m, the be full of cracks that then propagates into the 1st overlayer and then propagate into the middle layer might also occur in the outermost layer.If surpass 500 μ m, bad order then take place easily.
Outermost layer need be transparent, and here transparent is meant and reaches the transparent of this degree of state that can see the layer under it at least.As long as keep the transparency, just can be colored, but most preferably be water white.The preferred transmittance in the visible region of the transparency is more than 50%.
As the 1st overlayer, the middle layer of setting, and the combination of transparent outermost preferable material as required, the combination that can enumerate epoxy resin (the 1st overlayer), epoxy resin (middle layer) and Oppanol (transparent outermost layer).
Next, to inspection of cracking of the present invention is described with covering the operation that is used for structure.At first, in forming the 1st tectal resin combination, mix the micro-capsule that contains cognitive liquid, modulate coating composition.Next, by brush etc. this liquid composition coating is formed on the surface that need carry out the structure of inspection of cracking.In addition, above-mentioned liquid composition, just has no particular limits so long as can not destroy the coating process of the micro-capsule that has mixed to the coating of bur structure.
Next, modulation in advance is used for forming the 2nd tectal resin combination, and said composition is overlapping and be coated with the 1st overlayer that forms as mentioned above, forms the 2nd overlayer.Comprise the 1st tectal each tectal coating process this moment, can use known method in the past such as brushing, roller coat, spraying.In addition, be under the situation of multilayer at the 2nd overlayer, can use the stacked repeatedly coating of said method.
As form the of the present invention the 1st and the resin combination of the 2nd tectal bonding agent in, only otherwise damage its original performance, can also cooperate known in the past adjuvant as required in addition.For example, under the situation that the material that structure is got rusty easily by iron etc. constitutes, can add rust preventive etc.
As the structure among the present invention, can enumerate easily and produce the metallic structure of be full of cracks because of metal fatigue, metal structures such as boats and ships, bridge, vehicle, aircraft, Work machine for example, but for example, as described in No. the 3329029th, patent, enclose the particle diameter of the micro-capsule of cognitive liquid by suitable selection, also can be used for concrete construction, equally also can be used for various reinforced plastics system structures.
In the present invention; on the 1st tectal surface that is dispersed with the micro-capsule that includes cognitive liquid; stacked outermost layer is transparent and have the 2nd a flexible overlayer; even therefore produce be full of cracks on the surface of bur (metallic structure or concrete construction); because outermost layer has flexibility; therefore be full of cracks can not propagate into outermost layer; so the cognitive liquid that flows out from the 1st tectal micro-capsule can not flow to tectal outside; and be detained protection in overlayer by the 2nd tectal hyaline layer; therefore improved the water tolerance/water proofing property of cognitive liquid, guaranteed identification for a long time according to the be full of cracks place of cognitive liquid.
Embodiment
Embodiment 1~5 and comparative example 1
The manufacturing of capsule: in azo based dye (Orient chemical company system) 100 weight portions, add the oleic acid of 5500 weight portions and stir making cognitive liquid (azo based dye: solvent=1: 55).In addition, the gelatin (city wall chemistry system breaking down intensity (bloom strength) 320) of 450 weight portions is put in the water of 3600 weight portions, 45 ℃ of following stirring and dissolving.Stir this solution on one side,, cognitive liquid is disperseed Yi Bian drop into above-mentioned cognitive liquid.Next, the gum arabic (with the pure medicine system of light) of 450 weight portions is put in the water of 3600 weight portions,, filtered and remove after the insolubles, put in the above-mentioned dispersion liquid 45 ℃ of following stirring and dissolving.Next, water 9000 weight portions that are heated to 45 ℃ are joined in the above-mentioned dispersion liquid.Afterwards, the acetic acid of use 15% adjusts to 4.9 with the pH value of dispersion liquid.Dispersion liquid is cooled to after 10 ℃, adds 25% glutaraldehyde solution (with the pure medicine system of light), 200 weight portions, and at room temperature stir about is 8 hours, obtains the micro-capsule slip.It is carried out filtration drying, obtain micro-capsule.Mean grain size is about 115 μ m.
Coatingization:, mix bi-component (two-component) epoxy coating that is mixed with this agent (main agent) rigidizer (Chinese paint company system EPICON T-500 whitewash) of 400 weight portions with respect to resulting micro-capsule 100 weight portions of drying.In addition, this agent is added 340 weight portions and 60 weight portions respectively with rigidizer, is pre-mixed (the 1st overlayer coating below is called and contains the micro-capsule epoxy coating).
(embodiment 1)
Evaluation test is with the making of test film: use brush, be coated on the micro-capsule compo that mixes as implied above in aluminum-magnesium series alloy (JIS-A5083P-O) the system treadmill test sheet (with reference to Fig. 1) and make its sclerosis, form the 1st overlayer.Next, on the 1st overlayer, use the brush coating not contain the bi-component epoxy coating China paint company system EPICON T-500 whitewash of above-mentioned micro-capsule) and make its sclerosis (the 2nd tectal middle layer).Dried coating thickness is 100~150 μ m (totals in the 1st overlayer and the 2nd tectal middle layer).And then as transparent outermost overlayer (the 2nd tectal hyaline layer), using brush coating isobutylene is rubber coating (the system TB1171 of Three Bond Co., Ltd.), and dry solidification.Coating thickness after the curing is 30~100 μ m (only hyaline layers).
(embodiment 2)
Except the 2nd tectal middle layer is not set, with the embodiment 1 the same test film of making.
(embodiment 3)
Except using styrene-butylene is that rubber coating (the system TB2093B of Three Bond Co., Ltd.) is as the outermost overlayer (the 2nd tectal hyaline layer), with the embodiment 1 the same test film of making.
(embodiment 4)
The 2nd tectal middle layer is not set, and use styrene-butylene be rubber coating (the system TB2093B of Three Bond Co., Ltd.) as outermost overlayer (the 2nd tectal hyaline layer), in addition, with the embodiment 1 the same test film of making.
(embodiment 5)
The manufacturing of capsule: in nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) in 100 weight portions, add the oleic acid of 5500 weight portions and stir making cognitive liquid (nigrosine based compound: solvent=1: 55).In addition, the gelatin (city wall chemistry system breaking down intensity 320) of 450 weight portions is put in the water of 3600 weight portions, 45 ℃ of following stirring and dissolving.Stir this solution on one side,, cognitive liquid is disperseed Yi Bian drop into above-mentioned cognitive liquid.Next, the gum arabic (with the pure medicine system of light) of 450 weight portions is put in the water of 3600 weight portions,, filtered and remove after the insolubles, put in the above-mentioned dispersion liquid 45 ℃ of following stirring and dissolving.Next, water 9000 weight portions that are heated to 45 ℃ are joined in the above-mentioned dispersion liquid.Afterwards, the acetic acid of use 15% adjusts to 4.9 with the pH value of dispersion liquid.Dispersion liquid is cooled to after 10 ℃, adds 25% glutaraldehyde solution (with the pure medicine system of light), 200 weight portions, and at room temperature stir about is 8 hours, obtains the micro-capsule slip.It is carried out filtration drying, obtain micro-capsule.Mean grain size is about 115 μ m.Except using this micro-capsule, with the embodiment 1 the same test film of making.
(comparative example 1)
Except using transparent reactive amino formic ether is that coating (the system ThreeLongie A-850 of Three Bond Co., Ltd.) is as the outermost overlayer, with the embodiment 1 the same test film of making.
Evaluation test fatigue cracking progress test: be immersed in 3% artificial seawater (eight continent medicine systems at the above-mentioned test film that will have size shown in Figure 1 (mm), use AQUAMARINE) under the state in, be installed in electricity-liquid servo-type fatigue tester (Tianjin, island servo pulse device, dynamic capacity 10tonf) in, by load 0~1.6tonf, the repeated tensile load of pulsation fully of frequency 4Hz carries out the test of fatigue cracking progress.Continue to test, in test film, produce be full of cracks, and grow to the length (about 20~450,000 times of multiplicity) of 20mm degree, the outward appearance of visualization test portion.Its result is as shown in table 1.
The test method that the tectal physical property test 1 of outermost extends:
Test film is made: as shown in Figure 2, arranges 2 aluminium sheets (test film 2) (0.3 * 25 * 100mm), by brush coating formation tectal each coating of outermost and bi-component epoxy coating, carry out drying and obtain overlayer 1.The dry film thickness that forms tectal each coating of outermost is about 150 μ m.After at room temperature dry about 7 days,, measure the amount of tension that causes the fracture of filming by cupping machine tension test sheet.In addition, calculate the ratio of amount of tension by following formula.
The ratio of amount of tension=(forming outermost) ÷ (amount of tension of bi-component epoxy coating) by the amount of tension of each coating of rete
The result is presented in the table 1 in the lump.
The test method of tectal physical property test 2 bonding strengths of outermost:
Test film is made: by brush, the plate of making at 2 aluminium (JIS Al040P) (on 100 * 25 * 2mm), is coated with the above-mentioned bi-component epoxy coating that is mixed with this agent and rigidizer with the regulation mixing ratio, carries out drying.Be coated with tectal each coating of formation outermost on a slice plate therein by brush, horse back and another sheet plate are fitted afterwards, become test film.About additive method, test according to the tensile shear bonding strength test method of JIS K6850 bonding agent.
Table 1
Figure C20048001790100121
◎: expression color development fabulous zero: the expression color development is good *: expression color development bad (cognitive liquid losss)-: represent that undetermined maybe can't measure
Result according to experimental example 1~5, even destroy micro-capsule because of base material produces be full of cracks, cognitive liquid flows out, outermost transparent covering layer take place flexible owing to will be followed be full of cracks, the cognitive liquid that has flowed out is retained in the overlayer, therefore can be in water/use in the marine or position of drenching with rain, and can control cognitive liquid and run off and fade along with the time.In addition, be provided with coloured intermediate cover layer as the 2nd tectal situation under because the 1st intratectal micro-capsule is by hidden, therefore can improve visual attractive in appearance, by the color of appropriate combination cognitive liquid and the color in middle layer, can emphasize color development more, improve visibility.
In addition, can learn, though it is relevant with the kind of the employed resin combination that is used for the 1st overlayer and the 2nd overlayer (also comprising the middle layer), but the extension of outermost transparent covering layer is preferably 5mm above (even more ideal is more than the 10mm) substantially, in addition, the bonding force of preferably clear overlayer and the layer below it lower (2MPa is following).
Embodiment 6
In nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) in 100 weight portions, the oleic acid and the stirring that add 5500 weight portions, make cognitive liquid (nigrosine based compound: solvent=1: 55), in addition, the gelatin (city wall chemistry system breaking down intensity 320) of 450 weight portions is put in the water of 3600 weight portions, 45 ℃ of following stirring and dissolving.Stir this solution on one side,, cognitive liquid is disperseed Yi Bian drop into above-mentioned cognitive liquid.Next, the gum arabic (with the pure medicine system of light) of 450 weight portions is put in the water of 3600 weight portions,, filtered and remove after the insolubles, put in the above-mentioned dispersion liquid 45 ℃ of following stirring and dissolving.Next, water 9000 weight portions that are heated to 45 ℃ are joined in the above-mentioned dispersion liquid.Afterwards, the acetic acid of use 15% adjusts to 4.9 with the pH value of dispersion liquid.Dispersion liquid is cooled to after 10 ℃, adds 25% glutaraldehyde solution (with the pure medicine system of light), 200 weight portions, at room temperature stir about is 8 hours, obtains the micro-capsule slip.It is carried out filtration drying, obtain micro-capsule.Mean grain size is about 115 μ m.With respect to resulting micro-capsule 100 weight portions of drying, mix the bi-component epoxy coating that is mixed with this agent rigidizer (Chinese paint company system EPICON T-500 whitewash) of 400 weight portions.In addition, this agent is added 340 weight portions and 60 weight portions respectively with rigidizer, is pre-mixed.Use brush, the coating that is mixed is coated on aluminium sheet, and (Al040P:1 * 60 * 100mm) are gone up and are dry, as test film.Dried coating thickness is 200~350 μ m.
(embodiment 7)
About the blending ratio of cognitive liquid, with respect to the nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) 100 weight portions, oleic acid is 460 weight portions, in addition, with the embodiment 6 the same test films of making.(nigrosine based compound: solvent=1: 4.6)
(embodiment 8)
About the blending ratio of cognitive liquid, with respect to the nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) 410 weight portions, oleic acid is 150 weight portions, in addition, with the embodiment 6 the same test films of making.(nigrosine based compound: solvent=1: 0.37)
(embodiment 9)
About the blending ratio of cognitive liquid, with respect to the nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) 100 weight portions, bobbin oil is 260 weight portions, oleic acid is 200 weight portions, in addition, with the embodiment 6 the same test films of making.(nigrosine based compound: solvent=1: 4.6)
(embodiment 10)
About the blending ratio of cognitive liquid, with respect to the nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) 11 weight portions, oleic acid is 549 weight portions, in addition, with the embodiment 6 the same test films of making.(nigrosine based compound: solvent=1: 50)
(reference example 1)
About the blending ratio of cognitive liquid, with respect to the nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) 6 weight portions, oleic acid is 554 weight portions, in addition, with the embodiment 6 the same test films of making.(nigrosine based compound: solvent=1: 91)
(reference example 2)
About the blending ratio of cognitive liquid, with respect to the nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) 450 weight portions, oleic acid is 110 weight portions, in addition, with the embodiment 6 the same test films of making.(nigrosine based compound: solvent=1: 0.24)
(reference example 3)
As cognitive liquid, adding anthraquinone based compound (Orient chemical company system 1-amino-4-hydroxy-2 (4-n-nonyl phenoxy group) anthraquinone orchil) 110 weight portions and mineral oil 450 weight portions makes, in addition, with the embodiment 6 the same test films of making.
(reference example 4)
About the blending ratio of cognitive liquid, with respect to the nigrosine based compound (solvent black 7: central synthetic chemistry corporate system) 9.2 weight portions, oleic acid is 550.8 weight portions, in addition, with the embodiment 6 the same test films of making.(nigrosine based compound: solvent=1: 60)
(reference example 5)
As cognitive liquid, add anthraquinone based compound (OILBLUE5502 of this chemical industrial company blue dyes is arranged) 110 weight portions, toluene 225 weight portions and mineral oil 225 weight portions and make, in addition, with the embodiment 6 the same test films of making.
(reference example 6)
As cognitive liquid, adding anthraquinone based compound (OILBLUE5502 of this chemical industrial company blue dyes is arranged) 55 weight portions, azo based compound (OILYELLOW5001 of this chemical industrial company weld is arranged) 55 weight portions, toluene 225 weight portions and mineral oil 225 weight portions makes, in addition, with the embodiment 6 the same test films of making.
(reference example 7)
As cognitive liquid, add azo based compound (the system SOC-1-0092 of Orient chemical company orange) 110 weight portions and mineral oil 450 weight portions and make, in addition, with the embodiment 6 the same test films of making.
Test method 1:, in the part of the film coated surface of above-mentioned test film, cut out the otch that wide 1mm is following, be about 5cm by cutting machine.Destroyed and the color development of the micro-capsule of notch.
This test film is put in the weather meter (weather meter), observed the state that has passed through after 1000 hours.Observational technique is as described below.
Under about 1.5m of white in daytime (daylight white) fluorescent light (40W * 2), place test film, above the test film and under about 45 ℃ from about 1m apart from the viewing test sheet.The result is as shown in table 2.
Table 2
◎: can easily confirm color
Zero: can confirm color
△: confirm difficulty slightly
*: can't confirm color (fading)
(embodiment 11)
(central portion of Al040P:1 * 60 * 100mm) is cut a kerf etc. to employed aluminium sheet in embodiment 6, process aluminium sheet to such an extent that be easy to bend to doubling, use brush, with the epoxy of being modulated among the embodiment 6 that contains micro-capsule is that cold coating is coated on and does not have the face of otch side, and make that dried coating thickness is 200~350 μ m, carry out drying and make 10 test films.
Is center curvature 90 degree with above-mentioned test film with above-mentioned notch, make coated face in the inboard and the outside respectively have 5, its result, no matter which test film, near its kink film coated surface has all produced the wire be full of cracks, can confirm to be accompanied by the breakage of micro-capsule, the nigrosine based compound flows out and causes color development.
Can learn from the result of embodiment 6~10,, compare, significantly improve against weather, thereby can carry out long Visual Confirmation with other dyestuffs if use the nigrosine based compound as the dyestuff that includes in the micro-capsule.

Claims (6)

1. the inspection of cracking of a structure is with covering, its surface at structure forms the overlayer that is dispersed with the micro-capsule of having enclosed cognitive liquid, when producing be full of cracks in this structure, this be full of cracks is transferred to this overlayer, micro-capsule in this overlayer is destroyed thereupon, the be full of cracks of the cognitive liquid that from this micro-capsule, flows out in overlayer, arrive cover surface, the be full of cracks that so can detect this structure produces, wherein, be dispersed with on this overlayer of this micro-capsule, at least 1 layer the 2nd overlayer that does not contain micro-capsule is set, simultaneously, the 2nd overlayer has transparent outermost, and described outermost layer has enough flexibilities and has when producing be full of cracks in the overlayer of micro-capsule at this with box lunch that it can not produce be full of cracks yet.
2. the inspection of cracking of structure as claimed in claim 1 is used and is covered, wherein,
More than 17 times of elongation of the layer beyond the outermost layer when this outermost elongation has the layer that exists in the overlayer of micro-capsule and the 2nd overlayer beyond the outermost layer for this.
3. the inspection of cracking of structure as claimed in claim 1 or 2 is used and is covered, wherein,
The cognitive liquid of being enclosed in this micro-capsule is a principal ingredient with nigrosine based compound and solvent, and its weight rate is the nigrosine based compound: solvent=1: 55~1: 0.37.
4. the inspection of cracking of structure as claimed in claim 1 or 2 is used and is covered, wherein,
The 2nd tectal outermost layer and the shear bond power between the overlayer under the outermost layer are below the 1MPa.
5. the inspection of cracking of structure as claimed in claim 1 is used and is covered, wherein,
The 2nd overlayer is by being painted to opaque interlayer and transparent outermost layer constitutes.
6. the inspection of cracking of structure as claimed in claim 1 is used and is covered, wherein,
This structure is the metallic structure.
CN200480017901A 2003-06-26 2004-06-24 Coating for inspection of cracking in structure Expired - Fee Related CN100580434C (en)

Applications Claiming Priority (3)

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JP2003181953 2003-06-26
JP055833/2004 2004-03-01

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JP6614938B2 (en) * 2015-11-27 2019-12-04 恵和株式会社 Multilayer sheet for crack detection, multilayer sheet roll for crack detection, manufacturing method of multilayer sheet for crack detection, wall surface processing method, and wall surface processed concrete structure
DE102016105147B4 (en) * 2016-03-21 2022-07-28 Knorr-Bremse Systeme für Nutzfahrzeuge GmbH Vehicle brake and braking system
CN110002809B (en) * 2019-04-04 2020-10-16 山东科技大学 Preparation method of concrete capable of reporting damage by self
CN116812800B (en) * 2023-08-30 2023-12-01 中国水利水电第七工程局有限公司 Slip form anti-cracking test control device, system and method

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