JPH0843324A - Flaw detecting agent for ceramics and method for detecting flaw - Google Patents

Abstract

PURPOSE:To effect the inspection with excellent discriminating property by using the crack detecting agent, which includes a specified quantity of each water soluble organic material, which is in the solid condition at the ordinary temperature and which is in the fluid condition at a specific temperature or higher, and a dye. CONSTITUTION:As the dye to be used, the water soluble dye such as acid dye, basic dye, direct dye, catalyst dye, reactive dye at 0.1-10% by weight in relation to the flaw detecting agent, desirably at 0.5-10% by weight, is used. As the water soluble organic material, which is in the solid condition at the ordinary temperature and which is in the fluid condition at 35 deg.C or higher, glycol such as polyethylene glycol, polypropylene glycol, polyoxyethylene fatty acid ester, fatty soap is used, and the surface active agent is desirably used. Quantity of addition of the water soluble organic material is 0.5-30% by weight in relation to the flaw detecting agent, and 3-30% by weight is desirable. The flaw detecting agent is obtained by mixing the dye, the water soluble organic material and water in a container, and heating and agitating them so as to be evenly dessolved. Adding order is arbitrary, and they can be added at the same time.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flaw detection agent and a flaw detection inspection method for detecting defects opened on the surface of a ceramic inspection object. In addition, in the present invention, a defect refers to a crack such as a crack or a hole which is opened on the surface of an inspection object.

[0002]

2. Description of the Related Art Conventionally, when inspecting for defects of ceramics used for electronic parts by using a penetrant inspection agent, it has been general that visual inspection of appearance is performed by a skilled worker. However, it is not easy to detect fine defects even by using a magnifying glass by visual inspection of the appearance by a skilled worker, and the method of using a microscope is inefficient. The conventional penetrant inspection method is to inspect the test object with a solvent-removable penetrant mainly composed of dye and organic solvent, or a washable penetrant mainly composed of dye, surfactant, water and organic solvent. After immersing the object, or by applying these penetrants to the inspection object to permeate the inside of the defect, and then wash and remove the excess penetrant adhering to the inspection object with an organic solvent or water, This is a method in which a white fine powder or a developer in which this is dispersed in a liquid is attached to an inspection object, and the penetrant liquid that has penetrated into the inside of the defect is drawn to the surface by a capillary phenomenon to form a pattern indicating the defect. In addition, the penetrant inspection method is classified into a fluorescent penetrant inspection method and a dye penetrant inspection method, depending on the observation method. The fluorescent penetrant inspection test method is a method in which a penetrant containing a fluorescent dye is used and the inspection object is irradiated with ultraviolet rays in a dark place to visually observe a pattern indicating a defect. The pattern has a wavelength of 550 when irradiated with ultraviolet rays.
Since it emits yellow-green fluorescence near nm, it can be clearly confirmed in a dark place. In order to carry out this method, it is necessary to make the test place dark and to use an ultraviolet irradiation device. Also,
The dye penetrant flaw detection test method is a method of visually observing using a penetrant liquid colored red under natural light or white light. Using this method, defects appear as a red pattern on the white developer coating, and a clear pattern is formed due to the contrast with the white background of the developer coating, making it possible to distinguish between defects and sound areas. Become. Therefore, in a bright place, the test can be performed indoors, outdoors, or day and night, and there is an advantage that no special device is required for performing the test.

In the flaw detection test of ceramics, since ceramics are often white, a washable dye penetrant for a dye penetrant flaw test is used as a penetrant, and a developing treatment with a developer, that is, white fine powder is omitted. Often. The reason is that the ceramics themselves have many fine holes, and therefore the ceramics themselves have the effect of sucking the permeate out of the defects and the expansion of the bleeding, without using the capillary action of the developer. The reason is that, since most of the ceramics are white, the defect indicating pattern by the penetrant can provide sufficient contrast. Further, when a developer is applied to ceramics, it becomes rather difficult to remove the white fine powder used in the developer. Since the above-mentioned water-washable dyeing penetrant must conform to the standards for penetrant flaw detection methods, while the penetrant is immersed in or applied to the defect of the inspection object (J
According to IS Z 2343, it is referred to as an infiltration time, and is defined as 5 minutes or more in the case of ceramics. ), It is composed of a solvent solution or a surfactant aqueous solution which is liquid at room temperature so as not to change physical properties such as viscosity. Therefore, even if the developer is not used, bleeding is not completely prevented, and bleeding cannot be controlled while having high defect detection sensitivity. Further, in a ceramic component having many slits (grooves) used in electronic components, it is inevitable that the penetrant remains in the slits even after cleaning.
When this is dried, the slits are indicated as red as well as defects, and the slits expand over time, and the entire ceramic becomes red. As a result, there is a problem that the appearance is not good, and finally, the dye is diffused to the sound part of the inspection object where the dye should not remain, so that the defect-free ceramic also becomes defective. Also, JP-A-60-1714
Japanese Patent Laid-Open No. 38-38 proposes a flaw detection method using an inspection liquid composed of an aqueous dye solution. However, this flaw detection method is a method of forming a defect indicator pattern by adsorbing a dye to the defect. Since there is almost no effect of expanding the defect indicator pattern, it is difficult to visually observe a fine defect of about 10 μm. is there. In addition, this method is composed of a permeation step and a drying step, and since it does not include a cleaning step, not only the defect of the inspection object but also the sound part is colored, not only the appearance is deteriorated, but also the dye remains. There is a problem that the dye remains on the sound part of the inspection object which should not be done.

[0004]

SUMMARY OF THE INVENTION The present invention solves the above problems in a ceramics flaw detection inspection method,
An object of the present invention is to provide a flaw detection inspection agent for ceramics and a flaw detection inspection method which have high defect detection sensitivity and prevent unnecessary bleeding from defects and are excellent in distinguishability between defects and sound portions.

[0005]

DISCLOSURE OF THE INVENTION The present invention relates to a flaw detection agent containing water as a main component of a solvent, which is a water-soluble organic compound which is 0.1 to 10% by weight of a dye and is solid at room temperature and fluid at 35 ° C. or higher. A flaw detector for ceramics containing 0.5 to 30% by weight of the substance, which is adhered to the surface of the inspection object of the ceramics, and the flaw is penetrated into the defects existing on the surface, A ceramic flaw detection method is characterized in that a flaw indication pattern is formed by washing the surface flaw detection agent with water and then heating and drying. In the present invention, when the flaw detection agent on the surface is washed with water and then dried by heating, the dye and the water-soluble organic substance that have penetrated into the defects ooze on the surface. When the heating is stopped and the temperature is returned to 35 ° C. or lower, the fluid organic substance is solidified and the surface bleeding stops. The present invention can control the bleeding of surface defects by the heating and drying time by utilizing this principle.

The reason why water is used as the main component of the solvent in the present invention is that a volatile organic solvent such as alcohol,
This is because when acetone or the like is used, the drying speed is so fast that unevenness of the test liquid is generated on the surface of the test object and a pseudo pattern is displayed, making it difficult to identify the defect. Also, when a non-volatile organic solvent such as phthalate is used, the test liquid drawn to the surface from the defect of the test object will be bleeding for a while due to the capillary action of the porous surface of the test object. Becomes larger with the lapse of time, and it becomes difficult to identify defects. In addition to preventing environmental deterioration and fire hazard due to the organic solvent, cost is also taken into consideration, and in the present invention, water is the main component of the solvent.

As the dyes which can be used in the present invention, water-soluble dyes such as acid dyes, basic dyes, direct dyes, mordant dyes and reactive dyes are used. Acid dyes include Acid Fast Orange SG, Brilliant Scarlet 3R, Ama
ranth, Acid Rhodamin B, Eosine G, Acid Milling Red
RS and the like. As a basic dye, Cation O
range G, Cation Pink FG, Methyl Violet, Crystal Vi
Examples include olet, Cation Red 6B and Rhodamin B.
Direct dyes include Direct Fast Orange S and Sirius Sup
ra Orange 2GL, Benzopurpurine 4B, Direct Fast Scar
Examples include let 4BS. Chrome as a mordant dye
Red B, Alizarine, Chrome Blilliant Red B, Chrome
Blilliant Violet R, Chrome Blilliant Violet B and so on. As a reactive dye, Procion Rubine B
Examples include S and Reactone Red 2B-F. In addition, a rust preventive, an antiseptic, an alcohol and the like can be added to the flaw detection agent of the present invention, if necessary. The amount of the dye used in the present invention is 0.1 to 10% by weight, preferably 0.5 to 10% by weight, based on the flaw detection agent. If it is less than 0.1% by weight, the defect indicating pattern becomes thin and sufficient contrast cannot be obtained, so that it is difficult to detect fine defects, which is not preferable. On the other hand, if it exceeds 10% by weight, not only the defect but also the sound part is colored because the color tone is too dark, the distinguishability between the defect and the sound part is deteriorated, and the solubility of the dye is deteriorated, which is not preferable.

As the water-soluble organic substance which can be used in the present invention and which is solid at room temperature and becomes fluid at 35 ° C. or higher,
Polyethylene glycol, polypropylene glycol,
Examples thereof include polyethylene oxide, polyoxyethylene alkylphenyl ether, sodium dioctylsulfosuccinate, polyoxyethylene fatty acid ester, polyoxyethylene fatty acid ether, sorbitan fatty acid ester, polyglycerin fatty acid ester, glycol such as fatty acid soap, and surfactant. Among these, especially when a surfactant is used, the flaw detection agent can be easily washed. The addition amount of the water-soluble organic substance of the present invention is 0.5 to 3 with respect to the flaw detection agent.
It is 0% by weight, preferably 3 to 30% by weight. 0.5
If it is less than 10% by weight, it is difficult to detect a fine defect of about 10 μm because the effect of magnifying the defect design pattern is weak. Further, if the content exceeds 30% by weight, the viscosity of the test liquid becomes high, so that not only it takes a long time for the test liquid to penetrate into the defects, but also it takes a long time to clean the surplus test liquid on the surface. I don't like performance.

The ceramic flaw detection agent of the present invention is obtained by placing a dye, a water-soluble organic substance and water in a container, heating and stirring the mixture to uniformly dissolve it. In this case, the order of adding the water-soluble organic substance and the dye does not matter, and they may be added simultaneously. When performing a flaw detection inspection of ceramics using the flaw detection agent for ceramics of the present invention, the temperature and time for heating and drying can be appropriately selected depending on the physical properties of the water-soluble organic substance used, but usually about 100 C for about 1-10 minutes.

[0010]

When the ceramic flaw detection agent of the present invention is used for flaw detection inspection of ceramics, it is possible to prevent unnecessary bleeding of the dye from the defect, so that the distinction between the defect and the sound portion is excellent, and the defect is easily detected. Can be detected.

[0011]

【Example】

[Flaw inspection method] 30 μm wide and 0.2 m deep as a test plate
m slit and a white ceramics plate (70 mm x 70 mm x 0.
5 mm) was used. After applying the flaw detection agent and allowing it to penetrate for 10 seconds, the water pressure is 2.5 kgf at a distance of 25 cm from the test plate.
/ Cm ² shower-like spray for 10 seconds, then 10
The test plate was dried with warm air of 0 ° C. for 2 minutes. In addition,
The heating and drying conditions are those selected by the preliminary test.
The pattern of defects on the dried white ceramics plate was visually observed to determine the defect detection power, the degree of bleeding, and the ease of washing with water. Defect detection power is about 10 μm in width, which is clearly confirmed by a clear red color against a white ceramic background.
Mark), and those that were unclear or could not be confirmed were determined to have a poor defect detection power (x mark). The degree of bleeding is good when the defect indicating pattern formed by the flaw detection agent drawn out from the slit or the defect does not contaminate the slit or the periphery of the defect even after 24 hours have passed (○ mark). Those that were contaminated with the dye were regarded as defective (marked with x). As for the water washability, the excess flaw detection agent can be washed and removed from the test plate by washing with a shower spray having a water pressure of 2.5 kgf / cm ² at a distance of 25 cm from the test plate for 10 seconds. Those that were found to be defective (marked with X).

Examples 1 to 6 9 g (3.0 parts by weight) of commercially available polyoxyethylene nonylphenyl ether having a melting point of 47 ° C. in a 1 liter container and Kayanol Red NBR (Nippon Kayaku Co., Ltd.) which is an acid dye 4.5 g (1.5 parts by weight) and water 286.
5 g (95.5 parts by weight) was added, and the mixture was well stirred by using an ordinary stirrer at 70 ° C. and 1500 RPM for 30 minutes to obtain a flaw detection agent for ceramics of the present invention. Hereinafter, the flaw detection agent having the composition shown in Table 1 was prepared by the same method, and the flaw detection inspection was performed by the above-described flaw detection inspection method. The results are shown in Table 1.

[0013]

[Table 1]

Comparative Examples 1 to 6 The flaw detection agents having the compositions shown in Table 2 were prepared in the same manner as in Examples, and the flaw detection test was conducted in the same manner as in Examples.
It was shown to.

[0015]

[Table 2]

From Table 1, the flaw detection agent of the present invention has a defect detection power,
Both the bleeding condition and the water rinsing property are good. On the other hand, the flaw detection agents of Comparative Examples 1, 2, 3 and 6 in Table 2 have good bleeding condition, but there are problems in defect detection power and water rinsing property. The flaw detection agents of Comparative Examples 4 and 5 had a poor bleeding condition.

Claims (2)

[Claims] 1. A flaw detection agent containing water as a main component of a solvent, which is 0.1 to 10% by weight of a dye and is solid at room temperature and is 35 ° C.
Water-soluble organic substance 0.5-30% by weight
A flaw detection agent for ceramics containing. 2. The flaw detection agent according to claim 1 is attached to the surface of a ceramic inspection object, the inspection solution is allowed to penetrate into defects existing on the surface, the surface inspection solution is washed with water, and then heated. A method for flaw detection of ceramics, characterized by forming an indicator pattern of defects by drying.