JP2015014503A - Interface evaluation method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an interface evaluation method which exhibits an action effect which is not exhibited in a prior art and excellent in practical utility.SOLUTION: Provided is the method for evaluating an interface between a substrate and a coating on a subject which is formed by forming the coating on a surface of the substrate made of metal or a synthetic resin material or the like. Spherical abrasive grains are injected with compressed air to the subject for reducing the subject. Then, based on a reduction amount of the subject and an abrasive grain amount or time required for reducing the subject, intensity of the interface between the subject and the coating is determined for evaluating the interface.

Description

  The present invention relates to an interface between a substrate and a film in a subject in which a film is formed on the surface of a substrate such as a metal material or a synthetic resin material, or a film in a subject in which a plurality of films are stacked on the substrate surface. It is related with the interface evaluation method of evaluating the interface between.

  Conventionally, for example, peeling has been proposed as a method for evaluating the characteristics of the interface between a base material and a film in a subject in which a film is formed on the surface of a metal product or synthetic resin product, but the film is too thin. If it is fragile or brittle, there is a problem that the peeling cannot be performed well and the evaluation accuracy is remarkably lowered, or the evaluation itself cannot be performed. In addition, there is scratch as another evaluation method. However, if the film is too thin, it becomes a numerical value of scratch destruction including the film itself and the base material, so that the strength of the interface itself cannot be measured. There is.

  Therefore, there is a demand for an interface evaluation method that can easily and satisfactorily evaluate the interface between the substrate and the film or the interface between the films even if the film formed on the substrate surface is thin.

  The present inventor has formed a plurality of coatings on the substrate surface or the interface between the substrate and the coating in the subject in which the coating is formed on the substrate surface such as the metal material and the synthetic resin material as described above. As a result, we developed an interface evaluation method with excellent practicality that exhibits unprecedented effects.

  The gist of the present invention will be described with reference to the accompanying drawings.

A method for evaluating an interface between a base material and a coating film in a subject in which a coating film is formed on the surface of a base material such as a metal material or a synthetic resin material, and injecting spherical abrasive grains together with compressed air onto the subject The subject is reduced, and the interface between the base material and the coating is expressed by the following equation 1 based on the causal relationship between the reduction amount of the subject and the amount or time of the abrasive grains required for the reduction. The interface evaluation method is characterized in that the interface is evaluated by knowing the strength of the interface.
Formula 1
Interfacial strength (wear rate ratio) = wear rate near the interface ÷ substrate and coating with higher wear rate

Further, it is a method for evaluating an interface between the films in a subject in which a plurality of films are laminated on a base material surface such as a metal material or a synthetic resin material, and spherical abrasive grains are put on the subject together with compressed air. The strength of the interface between the coatings from the following equation 2 based on the causal relationship between the amount of decrease in the subject and the amount or time of the abrasive grains required for the decrease. It is related with the interface evaluation method characterized by evaluating this and evaluating this interface.
Formula 2
Interface strength (ratio of wear rate) = wear rate near the interface ÷ surface film with a higher wear rate between the front and back surfaces

  Further, it is a method for evaluating an interface between the base material and the film in a subject in which a film is formed on the surface of the base material such as a metal material or a synthetic resin material, and spherical air grains are compressed on the subject. And the strength of the base material and the strength of the base material based on the causal relationship between the decrease amount of the subject and the amount or time of the abrasive grains required for the decrease. The present invention relates to an interface evaluation method characterized in that the interface is evaluated by knowing the thickness and the strength of the film.

  Further, it is a method for evaluating an interface between the films in a subject in which a plurality of films are laminated on a base material surface such as a metal material or a synthetic resin material, and spherical abrasive grains are put on the subject together with compressed air. The subject is reduced by jetting, and based on the causal relationship between the reduction amount of the subject and the amount or time of the abrasive grains required for the reduction, the strength in the vicinity of the interface and the interface as a boundary The present invention relates to an interface evaluation method characterized by evaluating the interface by knowing the strength of the front and back films.

  The interface evaluation method according to any one of claims 1 to 4, wherein the vicinity of the interface is a part of a predetermined range in a front and back direction with the interface as a boundary. is there.

  The interface evaluation method according to claim 1, wherein an abrasive having a maximum particle size of 10 μm or less is employed as the abrasive.

  The interface evaluation method according to any one of claims 1 to 6, wherein an abrasive having a Young's modulus of 300 GPa or less is employed as the abrasive.

  The interface evaluation method according to any one of claims 1 to 7, wherein an injection material in which the abrasive particles are mixed in a liquid is injected to the subject together with compressed air. It is concerned.

  Since the present invention has been described above, the interface evaluation method is excellent in practicality and can easily and satisfactorily evaluate the interface between the base material and the film or the interface between the films.

It is a table | surface which shows the process conditions of the conventional method which this inventor proposes. It is a graph which shows the interface evaluation result of the conventional method which this inventor proposes. It is a graph which shows the interface evaluation result of the conventional method which this inventor proposes. It is a table | surface which shows the process conditions of a present Example. It is a graph which shows the interface evaluation result of a present Example. It is a graph which shows the interface evaluation result of a present Example. It is a graph which shows the interface evaluation result of a present Example. It is a graph which shows the interface evaluation result of a present Example.

  An embodiment of the present invention which is considered to be suitable will be briefly described with reference to the drawings showing the operation of the present invention.

  The inventor has proposed a surface property evaluation method (hereinafter referred to as a conventional method) disclosed in Japanese Patent Application Laid-Open No. 2010-237071 in which abrasive grains are repeatedly injected onto a subject to reduce the amount.

  In other words, this conventional method is a technique for evaluating the strength of the material surface by applying abrasive particles to the surface of the subject to wear the surface and applying the fact that the wear progressing speed varies depending on the material strength. The abrasive is sprayed onto the subject to reduce the subject, and the causal relationship between the reduction in the subject and the amount of abrasive required for the reduction is confirmed to evaluate the surface characteristics of the subject. It is something that can be done.

  Since the present inventor can easily grasp the characteristics of each part in the depth direction of the subject with this conventional method, this conventional method has a film formed on the surface of a substrate such as a metal material or a synthetic resin material. It was considered that this method is effective as a method for evaluating the interface between a base material and a film in a subject, or the interface between films in a subject in which a plurality of films are laminated on the surface of the base material.

  However, when the interface evaluation was actually performed by the conventional method, it was found to be insufficient.

  That is, the interface is evaluated by spraying abrasive grains three times to a subject that has been coated with about 2 micrometers of color filter material 1, 2, 3 on the glass surface under the processing conditions shown in FIG. I tried.

  As can be seen from the graph of FIG. 2 based on the amount of abrasive grains and the wear depth, the part corresponding to the film (part where the graph line is steeply inclined) and the part corresponding to the base material (the graph line is It appears that the portion corresponding to the interface between the film and the substrate does not appear clearly, and therefore this interface cannot be evaluated well and cannot be adopted as an interface evaluation method.

  Also, in the graph of FIG. 3 shown based on the wear rate (wear depth / abrasive grain amount) and depth, there is an inclination between the portion corresponding to the film and the portion corresponding to the substrate. Although the part which seems to be an interface slightly appeared, it was still insufficient for evaluating the interface.

  This is because the vicinity of the interface (hereinafter referred to as the interface portion) in a predetermined range in the front and back direction with the interface as the boundary is extremely thin, and when the abrasive grains collide with this thin site, the site is immediately cut, and the graph I guessed that it would not appear in the.

  Therefore, the present inventor has conceived of adopting spherical abrasive grains. In other words, spherical abrasive grains have a weaker cutting action than square abrasive grains, and minute wear is removed due to fatigue, stretching, etc., and wear progresses slowly, thus suppressing cutting at the interface. Assuming that the difference in the progress of wear could be expanded, when spherical abrasive grains were jetted together with the compressed air, it was confirmed that a portion corresponding to the interface portion appeared in the graph.

  Specifically, the interface was evaluated by injecting abrasive grains three times to the same subject as in FIG. 2 under the processing conditions shown in FIG.

  As can be seen from the graph of FIG. 5 shown based on the amount of abrasive grains and the wear depth showing the result, the part corresponding to the coating (enclosed part B in FIG. 5) and the part corresponding to the substrate A part corresponding to the interface (enclosed part A in FIG. 5) appeared between (enclosed part C in FIG. 5).

  From the graph of FIG. 5, the portion corresponding to the interface is weaker than the other portions, and it can be seen at which depth position the interface is distributed.

  Further, in the graph of FIG. 6 shown based on the wear rate (wear depth / abrasive grain amount) and depth, the portion corresponding to the coating (enclosed portion B in FIG. 5) and the portion corresponding to the base material. A part corresponding to the interface (enclosed part A in FIG. 5) appeared between (enclosed part C in FIG. 5).

  From the graph of FIG. 6, the portion corresponding to the interface is weaker than the other portions, and it can be seen at which depth position the interface is distributed.

  Further, from the graph of FIG. 6, the wear rate ratio is defined as the strength of the interface, and it is confirmed that the strength of the interface can be evaluated by the ratio of the wear rate in the vicinity of the interface to the wear rate of the film or the substrate. Since the strength of the interface could be quantified, it was possible to compare the strength with other interfaces.

Specifically, the following formula 1 is found, the strength of the interface between the substrate and the film is calculated, and the interface between the substrate and the film can be evaluated. In practice, it is important that the strength of the interface is stronger or weaker than the weaker base material or film (higher wear rate), so that the denominator has the higher wear rate.
Formula 1
Interfacial strength (wear rate ratio) = wear rate near the interface ÷ substrate and coating with higher wear rate

  According to the above formula 1, the case where the interface strength is 1 can be evaluated as necessary and sufficient. When the interface strength is less than 1, the interface strength can be evaluated as strong. When the interface strength is greater than 1, the interface strength can be evaluated as weak. .

  Similarly to the case of evaluating the interface between the film and the substrate described above, when evaluating the interface between the films in a subject in which a plurality of films are laminated on the surface of the substrate, the wear rate ratio is defined as the strength of the interface. It was confirmed that the strength of the interface can be evaluated by the ratio of the wear rate in the vicinity of the interface to the wear rate of the coating on the front and back surfaces with the interface as the boundary. It is also possible to compare the strength of.

Specifically, the following formula 2 can be found, the strength of the interface between the films can be calculated, and the interface between the films can be evaluated. In practice, it is important that the strength of the interface is stronger or weaker than the weaker film (higher wear rate), so that the denominator has the higher wear rate.
Formula 2
Interface strength (ratio of wear rate) = wear rate near the interface ÷ surface film with a higher wear rate between the front and back surfaces

  According to the above formula 2, the case where the interface strength is 1 can be evaluated as necessary and sufficient. When the interface strength is less than 1, the interface strength can be evaluated as strong. When the interface strength is greater than 1, the interface strength can be evaluated as weak. .

  5 and FIG. 6, it can be seen at which depth position the interface is distributed, and further know how strong or weak the strength in the vicinity of the interface is compared with the film or the substrate. The interface with the film and the interface between the films can be evaluated.

  Therefore, it has been found that the use of spherical abrasive grains makes it possible to satisfactorily evaluate the interface between the film and the substrate and the interface between the films in the subject.

  The present invention has been created based on the above facts and results.

  Specific embodiments of the present invention will be described with reference to the drawings.

  In this example, the interface between a base material and a film in a subject in which a film is formed on the surface of a base material such as a metal material or a synthetic resin material, or in a subject in which a plurality of films are laminated on the surface of the base material A method for evaluating an interface between coatings, the evaluation device having the same structure as the evaluation device used in the conventional evaluation method including an injection unit that reduces the subject by injecting spherical abrasive grains together with the compressed air to the subject. This is the case where specially researched and developed abrasive grains are used.

  Specifically, using the apparatus and mechanism disclosed in Japanese Patent Application Laid-Open No. 2010-237071, spherical particles were used as the material for the spraying abrasive grains made of glass (SiO 2). The beads used had an average particle size of 1.0 μm and a Young's modulus of 94 GPa.

  As shown in the table of FIG. 4, the injection condition is to prepare a spray material (slurry) in which the glass beads are adjusted to 1 wt% in water, and this slurry is guided to the spray nozzle and mixed and accelerated with compressed air. Jetted. The pressure of the compressed air at this time was 0.25 MPa, the distance between the nozzle tip and the subject was fixed at 4 mm, and the injection angle was 90 °.

The subjects were three types of synthetic resin base materials (E48R (Optical resin manufactured by Nippon Zeon Co., Ltd.)), 330R (Optical resin manufactured by Nippon Zeon Co., Ltd.), Panlite (manufactured by Teijin Limited). (Registered trademark of polycarbonate resin)) and glass substrates were selected by coating thin and transparent inorganic titanium oxide (TiO ₂ ) with a thickness of 210 nanometers by EB (electron beam) method. .

  The procedure is to inject the amount of abrasive grain calculated from the slurry flow rate and measure the depth of the center of the wear mark with a precision shape measuring instrument (such as a stylus type or optical interference type shape measuring machine). The method of repeatedly performing this method (a method of obtaining correlation data between the amount of abrasive grains and the wear depth) was selected. A method of obtaining correlation data between time and wear depth may be used.

  FIG. 7 shows the relationship between the cumulative amount of abrasive grains obtained in the above test and the wear depth.

  A site (enclosed site A in FIG. 7) corresponding to the interface between the site corresponding to the film (enclosed site B in FIG. 7) and the site corresponding to the substrate (enclosed site C in FIG. 7) Appeared.

  From the graph of FIG. 7, the portion corresponding to the interface is weaker than the other portions, and it can be seen at which depth position the interface is distributed.

  Further, in the graph of FIG. 8 shown based on the wear rate (abrasion depth / abrasive grain amount) and the depth, the portion corresponding to the film (enclosed portion B in FIG. 8) and the base are also examined. A part corresponding to the interface (enclosed part A in FIG. 8) appeared between the part corresponding to the material (enclosed part C in FIG. 8).

  From the graph of FIG. 8, the portion corresponding to the interface is weaker than the other portions, and it can be seen at which depth position the interface is distributed.

  Further, from the graph of FIG. 8, the strength of the interface can be expressed by a numerical value in proportion to the strength of the film or the substrate.

Specifically, the strength of the interface between the substrate and the film can be calculated from the following formula 1 to evaluate the interface between the substrate and the film.
Formula 1
Interfacial strength (wear rate ratio) = wear rate near the interface ÷ substrate and coating with higher wear rate

  According to the above formula 1, a case where the strength degree is 1 can be evaluated as necessary and sufficient, and if it is smaller than 1, it can be evaluated as strong, and if it is larger than 1, it can be evaluated as weak.

  Specifically, the strength of the interface between the substrate and the coating in each material (E48R, 330R, Panlite (registered trademark), glass) using Formula 1 is as follows. Note that the wear rate in Equation 1 is the maximum wear rate.

  In the case of TiO2 EB E48R, the strength of the interface is the wear rate in the vicinity of the interface (0.046) ÷ the wear rate of the substrate (0.028) = 1.64.

  In the case of TiO 2 EB 330R, the strength of the interface is the wear rate in the vicinity of the interface (0.097) ÷ the wear rate of the substrate (0.040) = 2.43.

  In the case of TiO 2 EB Panlite (registered trademark), the strength of the interface is the wear rate in the vicinity of the interface (0.030) ÷ the wear rate of the substrate (0.008) = 3.75.

  In the case of TiO 2 EB glass, the strength of the interface is the wear rate in the vicinity of the interface (0.018) ÷ the wear rate of the substrate (0.009) = 2.00.

  From this result, the interface strength of each subject is 1.64 to 3.75 on the basis of the wear rate of the weaker base material or film, and is larger than 1, so that there is an interface with considerably weak interface strength. It can be seen that it exists.

  7 and 8, E48R, 330R and Panlite (registered trademark) include a part corresponding to the base material (enclosed part C in FIGS. 7 and 8) and a part corresponding to the interface (see FIG. 7). A portion (enclosed portion D) that is weaker than the portion corresponding to the base material and stronger than the portion corresponding to the interface portion appears between the surrounding portions A) in FIGS.

  The enclosed part D in FIGS. 7 and 8 is a part where the resin has been altered by the high energy of the EB deposition of the film, and it can be seen that there is a weak part with a considerable thickness. I understand that I can't see it.

  Thus, the state of each part in the depth direction of the subject can be evaluated easily and in detail.

  From the above, it was found that the interface between the base material and the film formed on the surface of the subject can be evaluated by using abrasive grains having a spherical diameter. In addition, it has also been found that the interface between coatings in a subject in which a plurality of coatings are formed on the substrate surface can be evaluated.

  That is, good evaluation could not be made with square abrasive grains, but when the amount of abrasive grains and wear depth were graphed using spherical abrasive grains, the interface state clearly appeared. Therefore, it was possible to evaluate the subject's interface well and to quantify it.

  Since the present Example was comprised as mentioned above, it becomes the interface evaluation method excellent in practicality which can evaluate easily the interface of a highly accurate membrane | film | coat and a base material.

  Specifically, it is possible to quantify the correlation between the two materials to be joined. Therefore, the peeling and adhesion strength of joint interfaces such as painting, plating, thin film coating (hard and soft), rubber and elastomer, In addition to quantifying the interface strength before and after fatigue, quantifying the interface strength before and after thermal history, and quantifying the interface strength before and after alteration (light and chemicals), the following effects can be expected.

(1) Refinement and sophistication of interface design / development can be expected.
(2) Expected to improve quality by quantification of material interface that could not be done before.
(3) Expected improvement in production technology assurance capability.
(4) Expected to improve quality by quantifying ultra-thin film interface.

  Note that the present invention is not limited to this embodiment, and the specific configuration of each component can be designed as appropriate.

Claims (8)

A method for evaluating an interface between a base material and a coating film in a subject in which a coating film is formed on the surface of a base material such as a metal material or a synthetic resin material, and injecting spherical abrasive grains together with compressed air onto the subject The subject is reduced, and the interface between the base material and the coating is expressed by the following equation 1 based on the causal relationship between the reduction amount of the subject and the amount or time of the abrasive grains required for the reduction. An interface evaluation method characterized in that the interface is evaluated by knowing the strength of the interface.
Formula 1
Interfacial strength (wear rate ratio) = wear rate near the interface ÷ substrate and coating with higher wear rate A method for evaluating an interface between the coatings in a subject in which a plurality of coatings are formed on a base material surface such as a metal material or a synthetic resin material, wherein spherical abrasive grains are jetted onto the subject together with compressed air. The subject is reduced, and the strength of the interface between the coatings is ascertained from the following equation 2 based on the causal relationship between the reduction amount of the subject and the amount or time of the abrasive grains required for the reduction. And evaluating the interface.
Formula 2
Interface strength (ratio of wear rate) = wear rate near the interface ÷ surface film with a higher wear rate between the front and back surfaces   A method for evaluating an interface between a base material and a coating film in a subject in which a coating film is formed on the surface of a base material such as a metal material or a synthetic resin material, and injecting spherical abrasive grains together with compressed air onto the subject The subject is reduced, and based on the causal relationship between the reduction amount of the subject and the amount or time of the abrasive grains required for the reduction, the strength in the vicinity of the interface, the strength of the base material, and An interface evaluation method characterized by evaluating the interface by knowing the strength of the film.   A method for evaluating an interface between the coatings in a subject in which a plurality of coatings are formed on a base material surface such as a metal material or a synthetic resin material, wherein spherical abrasive grains are jetted onto the subject together with compressed air. The subject is reduced, and based on the causal relationship between the reduction amount of the subject and the amount or time of the abrasive grains required for the reduction, the strength in the vicinity of the interface and the An interface evaluation method comprising evaluating the interface by knowing the strength of the film.   5. The interface evaluation method according to claim 1, wherein the vicinity of the interface is a portion in a predetermined range in a front-back direction with the interface as a boundary.   The interface evaluation method according to claim 1, wherein an abrasive having a maximum particle size of 10 μm or less is employed as the abrasive.   The interface evaluation method according to claim 1, wherein abrasive grains having a Young's modulus of 300 GPa or less are employed as the abrasive grains.   8. The interface evaluation method according to claim 1, wherein an injection material in which the abrasive grains are mixed in a liquid is injected together with compressed air onto the subject.

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