CN107782653A - The Statistical Measurement of Radial Void of the thermal barrier coating porosity and Size Distribution - Google Patents
The Statistical Measurement of Radial Void of the thermal barrier coating porosity and Size Distribution Download PDFInfo
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- CN107782653A CN107782653A CN201610792690.8A CN201610792690A CN107782653A CN 107782653 A CN107782653 A CN 107782653A CN 201610792690 A CN201610792690 A CN 201610792690A CN 107782653 A CN107782653 A CN 107782653A
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- thermal barrier
- barrier coating
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- stomata
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- 239000012720 thermal barrier coating Substances 0.000 title claims abstract description 50
- 238000009826 distribution Methods 0.000 title claims abstract description 29
- 238000005259 measurement Methods 0.000 title claims abstract description 13
- 239000011800 void material Substances 0.000 title claims abstract description 6
- 239000012925 reference material Substances 0.000 claims abstract description 15
- 230000011218 segmentation Effects 0.000 claims abstract description 8
- 238000004611 spectroscopical analysis Methods 0.000 claims abstract description 8
- 238000010408 sweeping Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 18
- 239000005030 aluminium foil Substances 0.000 claims description 9
- 230000004888 barrier function Effects 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 239000011135 tin Substances 0.000 claims 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 abstract description 6
- 230000000007 visual effect Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 description 19
- 238000000576 coating method Methods 0.000 description 19
- 238000004458 analytical method Methods 0.000 description 12
- 239000010410 layer Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 241001270131 Agaricus moelleri Species 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001956 neutron scattering Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The present invention relates to the thermal barrier coating porosity and the Statistical Measurement of Radial Void of Size Distribution, it is characterised in that including：Through thickness cross-section samples are intercepted to thermal barrier coating to be measured as plane to be checked；It is placed in after reference material is pasted on into the edge of the plane to be checked on sample platform of scanning electronic microscope, and the backscatter images contrast of surface sweeping Electronic Speculum and the segmentation threshold of stomata identification is set；Control the surface sweeping electron microscopic sample platform to move by energy disperse spectroscopy, set analyzed area to carry out the programming count of the porosity；The statistics of the porosity is imported in Matlab programs, thermal barrier coating inner air vent rate described in statistic of classification.The present invention uses ESEM Momentum profiles instrument, and carry out more visual fields in the analyzed area of setting scans one by one, and the contrast threshold value according to stomata is identified, measured.
Description
Technical field
The present invention relates to thermal barrier coating microstructure characterizations field, in particular it relates to a kind of thermal barrier coating porosity and chi
The Statistical Measurement of Radial Void of very little distribution.
Background technology
Ceramic base heat barrier coat material is widely used in the hot-end component of Aero-Space engine, turbine, steam turbine, can
The surface temperature of high temperature alloy is effectively reduced, so as to improve efficiency, reduce oil consumption, extension hot-end component life-span.And modern deep space
Big aircraft, the spacecraft of operation require that engine has more big thrust loading, therefore must just improve turbine inlet gas temperature, and it is crucial
It is the high-temperature resistance for improving the hot-end components such as engine chamber, turbo blade.Heat barrier coat material is then to solve this
The important channel of problem.Research shows the porosity of thermal barrier coating, especially Stomata Type, Size Distribution, has a strong impact on coating
Effect of heat insulation, the life-span, corrosion resistance etc..Therefore quick, accurate statistics measurement thermal barrier coating the porosity and Size Distribution tool
It is significant.
Stomata in thermal barrier coating has two kinds of a closed pore and open pore, therefore the porosity is held one's breath porosity, open pore
Point of rate and total porosity.The method of traditional measurement coating's air hole ratio mainly have weight method, mercury injection method, image analytical method and
Some other neutron scatterings and electrochemical method.But weight method can not measure pore size distribution；Mercury injection method can not be measured and closed
The porosity；Image method and some other method subjectivities are larger and be difficult experiment statisticses analysis so that data have larger random
Property and error.Therefore, a kind of quick, accurate, objective repeatable statistical measurement thermal barrier coating porosity and Size Distribution are developed
Method it is very necessary.
The content of the invention
In view of the problem present on, the technical problems to be solved by the invention are to provide a kind of measurement thermal barrier coating gas
The method of porosity and Size Distribution, its is simple to operate, result is accurate, repeatable, statistical significance is strong.
To solve the problems, such as that prior art is present, the statistics of the thermal barrier coating porosity provided by the invention and Size Distribution is surveyed
Amount method, including：
Through thickness cross-section samples are intercepted to thermal barrier coating to be measured as plane to be checked；
It is placed in after reference material is pasted on into the edge of the plane to be checked on sample platform of scanning electronic microscope, and surface sweeping Electronic Speculum is set
Backscatter images contrast and the segmentation threshold of stomata identification；
Control the surface sweeping electron microscopic sample platform to move by energy disperse spectroscopy, set analyzed area to carry out the programming count of the porosity；
The statistics of the porosity is imported in Matlab programs, thermal barrier coating inner air vent rate described in statistic of classification.
The present invention uses ESEM Momentum profiles instrument, and carry out more visual fields in the analyzed area of setting scans one by one, according to
It is identified, measures according to the contrast threshold value of stomata.The repeatable statistical measurement thermal barrier coating porosity of the present invention and Size Distribution, and
Open pore can be measured simultaneously, the information such as hole and Size Distribution of holding one's breath.
Preferably, it is carried out to inlay polishing after the through thickness cross-section samples are intercepted, it is to be measured so as to can ensure that
Surfacing, pollution-free, no marking.
It is preferred that divided into according to the average atomic number of the reference material and heat barrier coat material ratio in backscatter mode
The contrast of the surface sweeping Electronic Speculum is put, the contrast includes brightness and contrast.Preferably, it may be such that the reference material ash
Angle value is 20~40, and the gray value of the plane to be checked is 150~200.And then gas in thermal barrier coating can be set under this contrast
The segmentation threshold in hole.
It is preferred that the analyzed area is square analyzed area, the size of a side is in its length direction or width
The through thickness of the through thickness cross-section samples, the size of the opposing party are not less than 1mm.
It is preferred that the reference material is one kind in aluminium foil, copper foil, tinfoil paper.
It is preferred that according to average Feret's diameter, maximum and the minimum Feret's diameter ratio of measurement stomata, to the heat
Barrier coating inner air vent carries out statistic of classification.
It is preferred that according to the porosity in the unit area along the thermal barrier coating thickness direction, evaluate the thermal boundary and apply
The uniformity of gas cell distribution in layer.
According to the present invention, Stomata Type, the porosity, Size Distribution and the coating of thermal barrier coating can be counted in large area
The uniformity of inner air vent distribution, and the stomata measured includes open and close stomata.
Brief description of the drawings
Fig. 1 is thermal barrier coating polishing section and the lower back scattering shape of 200 times of reference material (aluminium foil) in one embodiment of the invention
Looks；
Fig. 2 is that thermal barrier coating amplifies 1000 times of back scattering patterns and stomata identification under Fig. 1 gray scales in the present embodiment；
Fig. 3 is X, the Y-coordinate distribution schematic diagram for counting stomata in the present embodiment in thermal barrier coating；
Fig. 4 a are thermal barrier coating porosity variance through-thickness distributing homogeneity statistical distribution in the present embodiment；
Fig. 4 b are thermal barrier coating porosity deviation through-thickness distributing homogeneity statistical distribution in the present embodiment；
Fig. 4 c are thermal barrier coating stomatal number through-thickness distributing homogeneity statistical distribution in the present embodiment.
Embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The method of the present invention has simple to operate compared with traditional porosity method of testing, and the degree of accuracy is high, repeatability is strong
The characteristics of, analysis result is simultaneously comprising open and close stomata in thermal barrier coating.Illustrate to following exemplary that thermal boundary provided by the invention applies
The Statistical Measurement of Radial Void of the layer porosity and Size Distribution.
Prepare thermal barrier coating through thickness Cross section polishing sample.The through thickness section of thermal barrier coating through thickness cross-section samples is entered
Row inlays polishing, it is ensured that smooth, the pollution-free, no marking of surface (plane to be checked) to be measured, and it is parallel with bottom surface.In addition, selection is just
True grinding and glossing, moreover it is possible to while avoid because of excessive projection, pit or the original form for tearing change stomata and crackle.
In the present invention, the thermal barrier coating for example can be ZrO2, but the invention is not restricted to this.
Set unified contrast (such as brightness, contrast) gentle under ESEM backscatter mode using reference material
The segmentation threshold of hole identification.Specifically, reference material (such as aluminium foil, copper foil, tinfoil paper are pasted on coating (plane to be checked) border
Deng), accelerating potential (10KV~25KV) is set；Electronic beam current ensures that the dead time of energy disperse spectroscopy is more than 40%.In backscatter images
Under pattern, select relatively low multiplication factor (such as 200 ×) that coating and aluminium foil are placed in same visual field, ESEM unification is set
Brightness and contrast's (for example, can be according to the average atomic number of aluminium foil and coating ratio) so that the reference material gray value is
20~40, the gray value of the plane to be checked is 150~200.Keep this contrast constant in subsequent survey.Under this contrast,
The segmentation threshold of setting heat barrier coat material and stomata, the preferably numerical value between reference material and coating gray value, such as 80~
100, it is ensured that the stomata in image is by accurate, all identification.
Further, present invention additionally comprises the average atomic number ratio according to reference material and thermal barrier coating, objective, standard
The brightness of setting ESEM, contrast, set stomata to identify on this basis, segmentation threshold so that result is repeatable strong.
Momentum profiles instrument sets analyzed area to carry out stomata programming count.Analyzed area is set, the whole of coating should be included
Thickness.According to the minimum dimension hole diameter to be detected, suitable multiplication factor is selected, it is typically chosen 1000 ×, (detection is minimum
0.5 μm of stomata, crack size).As far as possible high digital image resolution is selected on the basis of analysis time is taken into account.It is basic herein
On, energy disperse spectroscopy splits analyzed area automatically, one by one scanning analysis.
Further, the analyzed area may be configured as square region, and long (width) degree direction includes thermal barrier coating through thickness, separately
One direction is not less than 1mm so that result statistical significance is strong.
Result is imported in Matlab programs and analyzed.Maximum gauge according to stomata is classified with minimum diameter ratio
Statistics.By setting sample platform of scanning electronic microscope X, Y-coordinate selection analysis region, set suitable multiplication factor and carry out analyzed area
Average segmentation, stomata image recognition and constituent analysis are carried out using energy disperse spectroscopy.
Along coating layer thickness direction unit of account region inner air vent rate one by one, thermal barrier coating inner air vent distributing homogeneity is carried out
Evaluation.Statistical result is saved as in Excel, imported into Matlab processing softwares.Feret's diameter according to stomata respectively, most
Big and minimum diameter compares stomata and carries out statistic of classification.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by this paper explanation
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment：
Step 1：Cross-section samples are taken from Thermal Barrier Coating Layers Prepared By Plasma Spraying, long (width) degree includes coating through thickness 1mm, the opposing party
To 1mm.Through inlaying polishing, it is ensured that face to be checked is smooth and parallel with bottom surface.In the present embodiment, the thermal barrier coating is ZrO2。
Step 2：On the basis of step 1, to ensure good electric conductivity, polished surface can carry out evaporation conductive carbon
Film.It is placed in after reference material (such as aluminium foil) is pasted on into coating edge with conductive tape on sample platform of scanning electronic microscope, sets and accelerate
Voltage 15KV；Electronic beam current ensures that the energy disperse spectroscopy dead time is more than 45%.
Step 3：On the basis of step 2, under backscattered electron image pattern, selection multiplication factor 200 × will apply
Layer and aluminium foil are placed in same visual field, adjust the brightness and contrast of ESEM, and it is 40 to make aluminium foil gray value, coating gray value
For 200, as shown in Figure 1.Keep this contrast constant in subsequent survey.
Step 4：On the basis of step 3, analyzed area is set, the full depth of coating should be included.Foundation will detect
Minimum dimension hole diameter, select multiplication factor for 1000 ×, (detecting 0.5 μm of minimum stomata, crack size).Taking into account point
As far as possible high digital image resolution is selected on the basis of the analysis time.
Step 5：On the basis of step 4, energy disperse spectroscopy splits square analyzed area automatically, one by one scanning analysis.It is square
The length on one side of analyzed area is the through thickness 1mm of the thermal barrier coating through thickness cross-section samples, and the length of another side is
1mm.As shown in Figure 3, the X-axis coordinate for counting stomata is 2.0mm~3.0mm, and Y-axis coordinate is 0.2mm~1.2mm.
Step 6：On the basis of step 5, the initial data in analyzed area is stored as Excel forms.It imported into
Subsequent treatment is carried out in Matlab programs.
Step 7：On the basis of step 6, Feret's diameter, minimum and maximum diameter according to stomata compare thermal boundary and applied
Stomata in layer is classified：Circular stomata and interlayer stomata.Total porosity and all types of porositys in coating are calculated respectively, its
Calculation formula is P=SStomata/SAnalyzed area* 100%.
Also, step 8：Thickness direction of the analyzed area along coating is equidistantly divided, according to the method point of step 7
The porosity that Ji Suan be in per unit region.
Step 9：Error statistics and distributing homogeneity point are carried out to each layer porosity data being calculated in step 8
Analysis, is processed data into as shown in the table：
Step 10：The statistics that step 9 is obtained does following processing, is porosity variance S2(Pi) in different analysis areas
The distribution curve in domain.If the peak value of Non Apparent Abnormality, illustrate that the distribution of thermal barrier coating inner air vent is more uniform.If in the presence of one or more
Individual anomaly peak, then illustrate thermal barrier coating inner air vent skewness.Porosity deviation is done respectivelyWith stomatal number in not
With the distribution curve of analyzed area.In the case of skewness, if in a certain regionAppearance positive maximum, and stomata
Quantity is minimum, and illustrate that stomata is uneven is mainly caused by larger-size stomata be present.This explanation thermal barrier coating is in preparation process
The molten condition of middle spraying powder is poor, that is, the more particle not melted completely be present.Therefore the stomata provided according to the present invention
Uniform distribution statistics can provide scientific guidance for thermal barrier coating preparation technology.
Fig. 2 is that thermal barrier coating amplifies 1000 times of back scattering patterns and stomata identification under Fig. 1 gray scales in the present embodiment, from figure
2 understand that the black stomata in image can be identified accurately.
X, the Y-coordinate distribution schematic diagram of stomata are counted in Fig. 3 the present embodiment in thermal barrier coating, as can be seen from Figure 3 statistical regions
It is that coating layer thickness direction is 1mm along Y-axis, is that other direction is 1mm along X-axis.
Fig. 4 a are thermal barrier coating porosity variance through-thickness distributing homogeneity statistical distribution in embodiment, can from Fig. 4 a
Know the porosity skewness at different-thickness in coating.Fig. 4 b be in embodiment thermal barrier coating porosity deviation along thickness side
To distributing homogeneity statistical distribution, understood from Fig. 4 b it is higher close to the body portion porosity in coating, close to surface portion then gas
Porosity is relatively low.Fig. 4 c are thermal barrier coating stomatal number through-thickness distributing homogeneity statistical distribution in embodiment, it was found from Fig. 4 c
It is relatively low on the contrary close to body portion stomata quantity in coating, and it is higher close to surface portion stomata quantity.In summary analysis can
Know, the molten condition that coating's air hole ratio is evenly distributed mainly due to feeding powder in preparation process is poor, causes preparation to apply initial stage
A small amount of larger-size stomata be present close to the part of matrix in layer.
Above-described embodiment is not intended to limit the present invention for the present invention will be described in further detail
Protection domain, all within the principle of the present invention, any modification, equivalent substitution and improvements done etc. should be included in the guarantor of the present invention
Within the scope of shield.
Claims (7)
- A kind of 1. Statistical Measurement of Radial Void of thermal barrier coating porosity and Size Distribution, it is characterised in that including：Through thickness cross-section samples are intercepted to thermal barrier coating to be measured as plane to be checked；It is placed in after reference material is pasted on into the edge of the plane to be checked on sample platform of scanning electronic microscope, and surface sweeping Electronic Speculum is set Backscatter images contrast and the segmentation threshold of stomata identification；Control the surface sweeping electron microscopic sample platform to move by energy disperse spectroscopy, set analyzed area to carry out the programming count of the porosity；The statistics of the porosity is imported in Matlab programs, thermal barrier coating inner air vent rate described in statistic of classification.
- 2. according to the method for claim 1, it is characterised in that according to being averaged for the reference material and heat barrier coat material The contrast of the atomic number than setting the surface sweeping Electronic Speculum under backscatter mode, the contrast include brightness and contrast.
- 3. method according to claim 1 or 2, it is characterised in that the analyzed area is square analyzed area, its length The size of a side is the through thickness of the through thickness cross-section samples in direction or width, and the size of the opposing party is not less than 1 mm。
- 4. according to the method any one of claim 1-3, it is characterised in that the reference material is aluminium foil, copper foil, tin One kind in paper tinsel.
- 5. according to the method any one of claim 1-4, it is characterised in that straight according to the average Fei Leite of measurement stomata Footpath, maximum and minimum Feret's diameter ratio, statistic of classification is carried out to the thermal barrier coating inner air vent.
- 6. according to the method any one of claim 1-5, it is characterised in that according to along the thermal barrier coating thickness direction Unit area in the porosity, evaluate the uniformity of gas cell distribution in the thermal barrier coating.
- 7. according to the method any one of claim 1-6, it is characterised in that after the through thickness cross-section samples are intercepted Fine polishing is carried out to it.
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| CN109580455A (en) * | 2019-01-07 | 2019-04-05 | 东北大学 | A kind of system and method measuring copper foil porosity |
| CN113899763A (en) * | 2020-06-19 | 2022-01-07 | 上海梅山钢铁股份有限公司 | Method for detecting and analyzing small-size nonmetallic inclusions in steel by using scanning electron microscope |
| WO2024120071A1 (en) * | 2023-08-03 | 2024-06-13 | 广东省科学院新材料研究所 | Measurement method for porosity of irregular columnar structure of thermal barrier coating |
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