CN110632048A - Method for improving fluorescence transmittance of thermal barrier coating sprayed by plasma - Google Patents
Method for improving fluorescence transmittance of thermal barrier coating sprayed by plasma Download PDFInfo
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- CN110632048A CN110632048A CN201910888485.5A CN201910888485A CN110632048A CN 110632048 A CN110632048 A CN 110632048A CN 201910888485 A CN201910888485 A CN 201910888485A CN 110632048 A CN110632048 A CN 110632048A
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- 239000012720 thermal barrier coating Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000002834 transmittance Methods 0.000 title claims abstract description 11
- 239000002480 mineral oil Substances 0.000 claims abstract description 22
- 235000010446 mineral oil Nutrition 0.000 claims abstract description 22
- 238000000576 coating method Methods 0.000 abstract description 28
- 239000011248 coating agent Substances 0.000 abstract description 26
- 230000005855 radiation Effects 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 description 20
- 238000007654 immersion Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000000691 measurement method Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L5/00—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
- G01L5/0047—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes measuring forces due to residual stresses
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for improving the fluorescence transmittance of a thermal barrier coating sprayed by plasma, which comprises the steps of putting a thermal barrier coating sample sprayed by plasma into a container filled with mineral oil, putting the container into a vacuum equipment cavity, and then reducing the vacuum degree of the equipment cavity from standard atmospheric pressure to 10‑3Pa; maintaining the vacuum degree for 40-80min, and then increasing pressure to return to standard atmospheric pressure. According to the invention, mineral oil is immersed in the coating in vacuum, microcracks and holes in the coating are filled with the mineral oil, and the filled mineral oil can reduce the reflection loss of a fluorescent signal when the fluorescent signal penetrates out of the coating, so that the Cr content in the thermally grown oxide is finally improved3+Inversion of fluorescent signal in coatingThe intensity of the radiation.
Description
Technical Field
The invention belongs to the technical field of nondestructive testing of thermal barrier coatings, and particularly relates to a method for improving fluorescence transmittance of a thermal barrier coating sprayed by plasma.
Background
The working environment of the high-temperature components of aircraft engines and gas turbines is extremely harsh, subject to hot corrosion and high temperatures, in addition to the various stresses that vary greatlyThe thermal oxidation and the like, so that the coating of the thermal barrier coating on the surface of the high-temperature component is an important thermal protection technology for protecting the high-temperature alloy substrate from being damaged. However, the extreme service environment and the hierarchical thermal protection structure lead to a complex failure mechanism of the thermal barrier coating. Failure of the thermal barrier coating during service is manifested by debonding and spalling of the ceramic layer. The generation, evolution and release of residual stress in the coating have a crucial influence on the failure of the coating, and are the core of the failure mechanism research of the thermal barrier coating. Therefore, there is a strong need for a non-destructive inspection technique that provides residual stress in the coating and that can assess the remaining life of the coating. At present, the fluorescence measurement method based on the elastic stress luminescence property of the rare earth elements has the incomparable advantages compared with the traditional measurement method, and special attention is paid to the fluorescence measurement method. The measuring method can realize the monitoring of the thermal growth oxide stress in the coating by doping the intelligent stress sensing material with elastic stress fluorescence characteristic in the material at the position to be measured. However, the method can only be used for thermal barrier coatings prepared by physical vapor deposition at present and cannot be used for coatings prepared by plasma spraying. This is because the plasma sprayed coating has a relatively loose structure with many holes and microcracks, which greatly weakens the Cr content in the thermally grown oxide3+The penetration of the fluorescent signal in the coating, and the thicker the coating, the more difficult it is for the fluorescent signal to pass through the overlying coating.
Disclosure of Invention
In order to solve the problem that a fluorescent signal is more difficult to penetrate through an upper coating in the prior art, the invention provides a method for improving the fluorescent transmittance of a thermal barrier coating sprayed by plasma, and the method has great significance for detecting the stress of a thermally grown oxide in the thermal barrier coating and evaluating the residual life of the coating.
The invention is realized by adopting the following technical scheme:
a method for improving the fluorescent transmittance of thermal barrier coating sprayed by plasma includes such steps as putting the specimen of thermal barrier coating sprayed by plasma in a container containing mineral oil, putting the container in the cavity of vacuum equipment, and lowering the vacuum degree of the cavity from standard atmospheric pressure to 10-3Pa; at the position ofMaintaining the vacuum degree for 40-80min, and then increasing the pressure to return to the standard atmospheric pressure.
The invention is further improved in that the vacuum degree of the equipment cavity is reduced to 10 from the standard atmospheric pressure by using a vacuum pump-3Pa。
A further development of the invention consists in returning to normal atmospheric pressure at a rate of pressure increase of 300 Pa/min.
The invention has the following beneficial technical effects:
according to the invention, mineral oil is immersed in the coating in vacuum, microcracks and holes in the coating are filled with the mineral oil, and the filled mineral oil can reduce the reflection loss of a fluorescent signal when the fluorescent signal penetrates out of the coating, so that the Cr content in the thermally grown oxide is finally improved3+The intensity of the reflection of the fluorescent signal in the coating. This is due to the fact that the refractive indices of air and coating are 1.0 and 2.7, respectively, and the refractive index mismatch is 1.7, the reflection loss of the fluorescence signal is relatively large when it passes through the coating/air interface. The refractive index of the mineral oil is 1.5, and the reflection loss of a coating/mineral oil interface is small, so that the light transmittance of the plasma sprayed coating is improved, and the maximum thickness can reach 400 mu m. Meanwhile, the mineral oil is hydrocarbon, so that the mineral oil can be decomposed into carbon dioxide and water vapor to be volatilized at high temperature only by carrying out high-temperature treatment once after measurement is finished each time in the actual use process, and the secondary service and nondestructive measurement of the coating can not be influenced. Other materials that reduce interfacial reflection losses and are highly removable may improve the optical transmission of the thermal barrier coating, such as epoxy.
Drawings
FIG. 1 shows Cr in thermally grown oxide3+Schematic diagram of fluorescence signal acquisition.
FIG. 2 shows Cr in thermally grown oxide3+A fluorescence signal profile.
FIG. 3 shows a degree of vacuum of 10-3Pa, Cr before and after impregnation3+Fluorescence signal intensity vs.
FIG. 4 shows a degree of vacuum of 100Pa, Cr before and after impregnation3+Fluorescence signal intensity vs.
FIG. 5 shows a degree of vacuum of 101Pa, Cr before and after impregnation3+Fluorescence signal intensity vs.
FIG. 6 shows a degree of vacuum of 102Pa, Cr before and after impregnation3+Fluorescence signal intensity vs.
FIG. 7 shows a degree of vacuum of 104Pa, Cr before and after impregnation3+Fluorescence signal intensity vs.
FIG. 8 is a graph showing Cr as the vacuum degree increases3+And (3) a change trend graph of the fluorescence signal intensity enhancement value.
Detailed Description
The invention is further described below with reference to the following figures and examples.
The invention provides a method for improving the fluorescence transmittance of a thermal barrier coating sprayed by plasma, which comprises the steps of putting a thermal barrier coating sample sprayed by plasma into a container filled with mineral oil by adopting vacuum equipment, putting the container into a cavity of the vacuum equipment, and then reducing the vacuum degree of the cavity of the equipment from standard atmospheric pressure to 10-3Pa; the vacuum was maintained for 40-80min and then returned to normal atmospheric pressure at a pressure rise rate of 300 Pa/min. Obtaining Cr in thermally grown oxides before and after impregnation3+694.3nm fluorescence signal intensity and comparison.
Specific examples of increasing the light transmittance of the coating are as follows:
the first step is as follows: selecting 5 groups of vacuum degree values which are respectively 104Pa、102Pa、101Pa、100Pa and 10-3Pa；
The second step is that: oxidizing the sample at 1150 ℃ for 40h to form a thermally grown oxide;
the third step: grinding and polishing the surface of the sample to ensure that the thickness of the coating is about 300 mu m;
the fourth step: cutting the sample into 5 small blocks, marking, and respectively corresponding to a vacuum degree;
the fifth step: cr before mineral oil immersion of the samples3+Obtaining the 694.3nm fluorescence intensity;
and a sixth step: carrying out vacuum impregnation on the samples under the conditions of 5 different vacuum degrees;
the seventh step: cr after mineral oil impregnation of test specimens3+Obtaining the 694.3nm fluorescence intensity;
eighth step: and processing the data to draw a conclusion.
Referring to FIGS. 1 and 2, FIG. 1 shows the detection of Cr in TGO layer of plasma sprayed coatings under excitation of 532nm excitation light3+The reflected fluorescence signal of (a) is a ceramic layer, b is a thermally grown oxide layer, and c is a metal substrate. FIG. 2 shows Cr in TGO3+Characteristic of fluorescence signal of, Cr3+Two peak positions, 694.3nm and 692.9nm respectively, are generated under the excitation of the exciting light. As can be seen from FIG. 2, Cr3+The most preferred emission peak position of (2), i.e., the maximum intensity of the reflected fluorescence signal, is 694.3nm, and therefore, the increase in Cr is expected3+In the experiment of fluorescence transmittance, the intensity of reflected fluorescence at 694.3nm will be measured.
Referring to FIG. 3, FIG. 3 shows a vacuum level of 10-3Before and after mineral oil immersion in Pa, Cr in TGO layer3+694.3 nm. Dotted line is Cr before impregnation3+The curve of the reflected fluorescence intensity of (2) shows an intensity at 694.3nm of almost 0. The 694.3nm intensity after impregnation is much increased, not only the peak position can be clearly shown, but also the intensity is increased by about 10000 counts.
Similar to FIG. 3, FIG. 4 shows a vacuum level of 100a, before and after mineral oil immersion, Cr in TGO layer3+694.3 nm. Dotted line is Cr before impregnation3+The curve of the reflected fluorescence intensity of (2) also shows an intensity of 0 at 694.3 nm. The 694.3nm intensity after impregnation is much higher, and not only the peak position can be clearly shown, but also the intensity is increased by about 8000 counts.
Referring to FIG. 5, FIG. 5 shows a vacuum level of 101a, before and after mineral oil immersion, Cr in TGO layer3+694.3 nm. Dotted line is Cr before impregnation3+The reflected fluorescence intensity curve of (2) shows a slight peak pattern at 694.3nm and the intensity is not 0. The 694.3nm intensity after impregnation is much increased, not only the peak position can be clearly shown, but also the intensity is increasedAbout 3000counts are obtained.
Referring to FIG. 6, FIG. 6 shows a vacuum level of 102a, before and after mineral oil immersion, Cr in TGO layer3+694.3 nm. Dotted line is Cr before impregnation3+The curve of the reflected fluorescence intensity of (2) shows an intensity at 694.3nm of almost 0. The 694.3nm intensity after impregnation is much increased, not only is the peak position clearly visible, but the intensity is increased by about 2000 counts.
Referring to FIG. 7, FIG. 7 shows a vacuum level of 104a, before and after mineral oil immersion, Cr in TGO layer3+694.3 nm. Dotted line is Cr before impregnation3+The curve of the reflected fluorescence intensity of (2) also shows an intensity at 694.3nm of almost 0. The 694.3nm intensity after impregnation is much increased, not only is the peak position clearly visible, but the intensity is increased by about 2500 counts.
Referring to FIG. 8, FIG. 8 shows Cr after mineral oil vacuum impregnation3+694.3nm and different vacuum degrees. It can be seen that the impregnation effect is most pronounced under high vacuum. As the vacuum degree is increased, the fluorescence intensity enhancement value is sharply reduced and then slowly reduced, and finally, the fluorescence intensity enhancement value is basically kept unchanged. Therefore, the most significant degree of vacuum for the dipping effect was 10-3Pa。
Claims (3)
1. A method for improving fluorescence transmittance of thermal barrier coating sprayed by plasma is characterized in that a thermal barrier coating sample sprayed by plasma is placed into a container filled with mineral oil, the container is placed into a vacuum equipment cavity, and then the vacuum degree of the equipment cavity is reduced from standard atmospheric pressure to 10-3Pa; maintaining the vacuum degree for 40-80min, and then increasing pressure to return to standard atmospheric pressure.
2. The method of claim 1, wherein the vacuum pump is used to reduce the vacuum of the chamber from a standard atmospheric pressure to 10 degrees f-3Pa。
3. The method of claim 1, wherein the pressure is increased at a rate of 300Pa/min to normal atmospheric pressure.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0552735A (en) * | 1991-08-23 | 1993-03-02 | Nippon Nuclear Fuel Dev Co Ltd | Method for measuring density distribution of powder compact |
| CN101768714A (en) * | 2010-02-09 | 2010-07-07 | 江苏大学 | Method for preparing thermal barrier coating by laser compound plasma spraying |
| KR20130061224A (en) * | 2011-12-01 | 2013-06-11 | 한국원자력연구원 | Vacuum desiccator for infiltration with epoxy resin of unconsolidated material |
| CN105132908A (en) * | 2015-10-16 | 2015-12-09 | 广东电网有限责任公司电力科学研究院 | Gas turbine blade thermal barrier coating bonding layer and preparation method thereof |
| CN108179373A (en) * | 2017-12-27 | 2018-06-19 | 江苏奇纳新材料科技有限公司 | Gas turbine blades thermal barrier coating prepared by a kind of spraying method |
-
2019
- 2019-09-19 CN CN201910888485.5A patent/CN110632048A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0552735A (en) * | 1991-08-23 | 1993-03-02 | Nippon Nuclear Fuel Dev Co Ltd | Method for measuring density distribution of powder compact |
| CN101768714A (en) * | 2010-02-09 | 2010-07-07 | 江苏大学 | Method for preparing thermal barrier coating by laser compound plasma spraying |
| KR20130061224A (en) * | 2011-12-01 | 2013-06-11 | 한국원자력연구원 | Vacuum desiccator for infiltration with epoxy resin of unconsolidated material |
| CN105132908A (en) * | 2015-10-16 | 2015-12-09 | 广东电网有限责任公司电力科学研究院 | Gas turbine blade thermal barrier coating bonding layer and preparation method thereof |
| CN108179373A (en) * | 2017-12-27 | 2018-06-19 | 江苏奇纳新材料科技有限公司 | Gas turbine blades thermal barrier coating prepared by a kind of spraying method |
Non-Patent Citations (1)
| Title |
|---|
| K.W. SCHLICHTING: "Application of Cr3+ photoluminescence piezo-spectroscopy to plasma-sprayed thermal barrier coatings for residual stress measurement", 《MATERIALS SCIENCE AND ENGINEERING：A》 * |
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