Penetration agent for capillary luminescent flaw detection

FIELD: capillary luminescent flaw detection, possible use in aviation, automobile, shipbuilding and other branches of mechanical engineering, and also power engineering, chemical and nuclear industries for detection of surface defects, cracks, pores, foliating, abscesses, inter-crystallite corrosion and other defects of material discontinuity flaw type, primarily with small dimensions, in case of especially precise control of products.

SUBSTANCE: penetration agent includes organic phosphor, non-ionic surfactant and solvent, while as organic phosphor a mixture of phosphors from the class of coumarin colorants is used - mixture of donor-coumarin and acceptor-coumarin, as nonionic surfactant a specially defined substance is used, and as solvent a mixture of dibutyl phthalate and propylene carbonate is used with mass ratio ranging from 1:1,5 to 1:0,8. As donor-coumarin, 4-methyl-7-dethyl amine coumarin (K-47) may be used, and as coumarin-acceptor, at least one coumarin of yellow-green luminescence, with mass ratio ranging from 1,1:1 to 1,8:1.

EFFECT: increased sensitivity and reliability of flaw detection, while simultaneously reducing fire hazard and toxicity of used composition.

1 ex, 1 tbl

 

The invention relates to liquid penetrant inspection, in particular, compositions indicator of fluorescent penetrants used for fluorescent industrial control products responsible for the appointment of metal, non-porous ceramics and plastics class surface roughness Rz of 20 and above. The invention can be used in aviation, automobile, shipbuilding and other industries, as well as energy, chemical and nuclear industries for the detection of surface defects, cracks, pores, laminations, sinks, intergranular corrosion and other defects such as discontinuities of the material, mainly with small sizes, especially when precise control products.

At the modern level of development of techniques to increase the sensitivity of the indicator of fluorescent penetrants in the compositions used several phosphors, working on the principle of "cascade luminescence" due to intermolecular energy transfer of electronic excitation. When this phosphor-donor absorbs radiation in the field of radiation of the UV lamp used for inspection of parts during the inspection. The phosphor-acceptor, along with the absorption of radiation UV lamp absorbs the radiation of the phosphor-donor and emits in the region most sensitive to the human eye (yellow-green region is pectra). Thus even when using two phosphors increases the sensitivity of the method compared to using only a single phosphor. When using a single phosphor, on the one hand, a lot of light is lost due to incomplete overlap of the spectra of the lamp radiation and the absorption spectrum of the phosphor, on the other hand, is not optimum for the human eye field of radiation, as Sexawy shifts phosphors in the considered spectral region does not exceed, as a rule, 100 nm.

Known for fluorescent penetrant flaw detection, comprising a phosphor-donor and a fluorescent acceptor, the wetting - polietilenglikolya esters of monoethanolamide synthetic fatty acids, dicamillo, kerosene and dimethylphthalate (SU 1633803 A1, 23.04.1993 year). Known penetrant as phosphor-donor contains 4′,4′′-dicyan-2-diplomatischer-1,4-distyrylbenzene, and as phosphor-acceptor 1,5-diphenyl-3-(4-diplomatischer)-pyrazolin-Δ2with all these components take in a certain ratio. Known penetrant allows to detect defects with a small opening to 0.5 μm at offset luminescence in a more favorable region of the spectrum. However, when it is used, when high brightness is not achieved sufficient reliability villenadirector, due to the low reproducibility of the results. In addition, the composition has a high toxicity and Flammability.

Known for fluorescent penetrant liquid penetrant inspection, including organic phosphor consisting of a fluorescent donor and fluorescent acceptor -, nonionic surface-active agent (surfactant) and the solvent (SU 1221891 A1, 20.01.1997 year). In a known composition includes the following components at the following ratio (wt.%):

4-Methyl-7-diethylaminocoumarin (phosphor-donor)0,3-0,8
N-Phenyl-n-butylimide
4-methoxypropylamine acid
(phosphor-acceptor)1,5-2,0
The mixture monoalkylphenol esters
poly (ethylene glycol) C8-C10(SAS)4,5-5,5
N-Organic42-50
Kerosene6,0-8,0
DibutylRest

The minimum size of detectable defects 1-2 μm. The disadvantage of this structure is not very high intensity and brightness of penetrant on the defects after application of the developer, h is about due to insufficiently high quantum yield of luminescence of the phosphor-acceptor. The result is a lack of sensitivity and reliability of detection of defects and, in addition, the low reproducibility of the results, especially when detecting defects of various sizes. In the composition of the penetrant include surfactants containing phenolic fragments, which determines its toxicity, particularly in the decomposition of sewage. In addition, the presence in its composition of kerosene makes it fire, which limits its application in industry.

At the present level of technology required inspection of materials particularly high level of sensitivity, i.e. allowing to reliably detect defects disclosure of 1 μm or less. Moreover, it is also the task of reducing fire hazard and toxicity as used in the composition of penetrant materials and the penetrant in General.

The task of the invention to provide an indicator of penetrant fluorescent penetrant inspection, do not have the above disadvantages.

The technical result of the invention is to improve the sensitivity and reliability of defect detection, while reducing fire hazard and toxicity of the used composition.

The technical result is achieved by the fact that according to the invention for fluorescent penetrant liquid penetrant inspection is before the organic phosphor, nonionic surfactant and a solvent as the organic phosphor used a mixture of phosphors of the class coumarin dye is a mixture of coumarin coumarin donor and acceptor, as nonionic surfactants - Sintana ALM-10 with the following component ratio (wt.%):

A mixture of coumarin dyes0.5 to 1.2
Sintana ALM-1010-15
SolventRest

the solvent used is a mixture of dibutyl phthalate (DBP) and propylene carbonate (PC) mass ratio of from 1:1.5 to 1:0,8.

Only the above proposed structure for fluorescent penetrant flaw detection described above is a set of essential features, when used in radiography provides increased sensitivity and reliability of detection of defects, and also reduces the Flammability and toxicity,

As a coumarin donor can be used 4-methyl-7-diethylaminocoumarin (47), and coumarin-acceptor, at least one coumarin yellow-green fluorescence under optimal mass ratio of from 1.1:1 to 1.8:1.

Fewer coumarin dyes reduces chustvitelnos the ü of penetrant; a greater number of, on the one hand, does not dissolve in the mixture of solvent and PAVA, on the other hand (in case of dissolution), leads to an incomplete removal of the background when you wash the excess of penetrant in the control that cannot provide the technical result of the claimed invention.

As surface-active substances (surfactants) selected Sintana ALM-10 (TU 2483-064-05015207-99), which is an ethoxylated fraction of alcohols C12-C14with an average degree of oksietilirovannye equal to 10. The fatty alcohol ethoxylates according to the degree of impact on the body are 3 hazard class according to GOST 12.1.007. Unlike monoalkylphenol ethers of polyethylene glycol (used in the prototype), they do not contain phenolic fragments, making them less toxic, particularly in the decomposition of sewage. The flash point in an open crucible 220°C; ignition temperature not lower than 240°C.

Sintana ALM-10, on the one hand, contributes to better dissolution of phosphors, on the other reduces the wetting angle. Wetting angle mixture PC - DBPS in the ratio of 1:1 by volume is ˜30°. Wetting angle of this mixture with addition of 10 wt.% Cintanya ALM-10 is ˜18°.

The viscosity of this mixture is approximately 6.5 CPS (at 20°C.

The number of Cintanya ALM-10 penetrant m is nisei, than 10 wt.%, and more than 15 wt.%, is not possible to provide the above technical result.

A mixture of dibutyl phthalate and propylene carbonate charge / mass ratio of from 1:1.5 to 1:0.8 to. These ratios, as well as above the value of the quantity of nonionic surfactant - Cintanya ALM-10 penetrant, according to the invention allows, on the one hand, to maintain the desired surface tension of penetrant, respectively, provides the necessary fluidity, and, on the other hand, provide the ability to dissolve the required amount of phosphors. It is at the specified value to achieve the specified technical result.

Organic solvents used for the penetrants must have a high boiling point (above 200°C), low volatility, relatively low toxicity, in the desired proportions used to dissolve organic phosphors, viscosity 2-6 CPS (at 20°and a surface tension of about 20 DN/see the Last two parameters determine the fluidity (wetting angle) and the necessary penetrating properties of penetrant. Given the above requirements, as an organic solvent was selected mixture of dibutyl phthalate and propylene carbonate.

Propylene carbonate (TU 2435-378-05742746-2001) high-boiling the content of inorganic fillers solvent with good solubility against organic phosphors. Boiling point 241°C. the degree of impact on the body propylene carbonate belongs to the 3rd class of hazard according to GOST 12.1.007. Flash point 126°C. the Autoignition Temperature of 485°C. wetting angle ˜40°.

Dibutyl phthalate (GOST 8728-88) - high-boiling organic solvent: boiling point 340°C (decomposition). The degree of impact on the body dibutyl applies to 2 hazard class according to GOST 12.1.007. However, the high boiling point and low volatility make possible its use in the inventive pentreath. Flashpoint 164°; auto-ignition temperature 400°C. wetting angle ˜20°.

The mass mixing ratio of phosphor-donor and phosphor-acceptor choose, using the known spectral properties of fluorescent donors and acceptors and given the required characteristics of resulting penetrant. For phosphors donors and acceptors from the class of coumarin dyes optimal from the point of view of intermolecular energy transfer is the ratio of from 1.1:1 to 1.8:1, which is obtained experimentally. The proposed coumarins-acceptors yellow-green fluorescence have a high quantum yield of luminescence, and a bright yellow-green glow. Their combination with coumarin donor (47) further enhances the brightness on the ositelu in UV light after application of the developer when performing capillary control, that increases the sensitivity of the method. The high absorption coefficient (εmax=5·104and the intensity of fluorescence (quantum yield of luminescence ϕ=0.6 to 0.8) in comparison with previously used in phosphors (derivative of naphthalimide), respectively having values εmax=5·103and ϕ=0,4-0,5, allows the use in the composition of smaller amounts of the phosphors. Due to different combinations of phosphors is possible to vary the concentration of the phosphors, the area of illumination and the sensitivity of penetrant.

Coumarin 47 and coumarins yellow-green glow of the degree of impact on the body belongs to the 3rd class of hazard according to GOST 12.1.007.

Table 1 shows the compositions of the claimed penetrants and prototype and testing results. The table shows the designation of coumarins according to the Handbook of laboratory reagents and equipment "Aldrich", except For 8. 8 is a 7-diethylamino-3-(benzoxazol-2-yl)coumarin.

The requested penetrants is obtained by mixing the component composition at 35-45°C.

An example implementation

Control was taken 4 metal sample with artificially caused by the defects corresponding to the first class of sensitivity according to GOST 18442-80, where

1st sample with defects opening width of 0.5 μm, a depth of 10 microns;

2nd sample with delectabilities disclosure of 1.0 μm, a depth of 20 microns;

3rd sample with defects opening width of 1.5 μm, a depth of 30 microns;

4th sample with defects opening width of 2.5 μm, a depth of 50 ám.

Specimens with artificial defects with opening width 2; 3; 5; 7; 8; 9; 10, the depth of 30-60 μm, the fragments of details with natural defects with a surface roughness Rz20√.

The control was carried out as follows.

On the precleaned surface of the samples was applied penetrant and kept for a certain period of time for penetration in his defects; then the excess penetrant from the surface washed with water. The samples were immersed in a bath of cleaning liquid coolant-7A (TU 2662-009-73057924-2004) and then washed in water. The last operation is required to remove the penetrant from the surface of the parts. The samples were wiped dry with a dry lint-free cloth, checked under UV light the completeness of the removal of excess penetrant (absence of yellow-green fluorescence) and using the paint sprayer inflicted developer PR-15A (TU 2662-011-73057924-2004) thin layer. Being part of the developer sorbent contributes to the fact that the remaining defects penetrant under the action of capillary forces comes to the surface and forms a flat drawings, y UV-rays. These figures correspond to defects on the surface of the parts. Ceres-40 minutes conducted the examination of samples in a darkened room under UV light and an assessment of the sensitivity. Traces of defects glowed a bright yellow-green. After controlling for the developer removed from the surface of the parts washing water at a temperature of 30-35°C.

The testing results show that the proposed fluorescent penetrant for liquid penetrant inspection has low volatility and low Flammability (flash point above 126° (C), less toxicity, particularly high sensitivity, provides a bright yellow-green glow in the defects (in the area most sensitive to the human eye)ensures the reproducibility of testing results at 99%, with a minimum width of detected defects is 0.5-1 μm. In control technology with the claimed penetrants used more easily removed from the developer. All these data allow us to extend the scope of application of penetrant, make its use more sophisticated.

Thus, the above and a reasonable set of features of the present invention is necessary and sufficient to obtain a technical result when implementing the claimed invention.

For fluorescent penetrant liquid penetrant inspection, including organic phosphor, nonionic surface-active the substance and the solvent, wherein the organic phosphor used a mixture of phosphors of the class coumarin dye is a mixture of coumarin-coumarin donor and the acceptor, as the coumarin donor used 4-methyl-7-diethylaminocoumarin (47), and coumarin-acceptor, at least one coumarin yellow-green fluorescence, when the mass ratio of from 1.1:1 to 1.8:1, as nonionic surfactants, Sintana ALM-10, in the following ratio, wt.%:

A mixture of coumarin dyes0.5 to 1.2
Sintana ALM-1010-15
SolventRest

the solvent used is a mixture of dibutyl phthalate and propylene carbonate in a mass ratio of from 1:1.5 to 1:0,8.



 

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