CN104808016B - A kind of method of oxidation zirconium base thermal barrier coating grain form clear - Google Patents
A kind of method of oxidation zirconium base thermal barrier coating grain form clear Download PDFInfo
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- CN104808016B CN104808016B CN201510161679.7A CN201510161679A CN104808016B CN 104808016 B CN104808016 B CN 104808016B CN 201510161679 A CN201510161679 A CN 201510161679A CN 104808016 B CN104808016 B CN 104808016B
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Abstract
The invention discloses a kind of method of oxidation zirconium base thermal barrier coating grain form clear, heat etching experiment clear is carried out with different temperatures and soaking time by the burnishing surface of microstructure of plasma sprayed coating, farthest discloses the crystal habit after the flat solidification of molten drop.Utilize scanning electron microscope, determine the optimal thermal etching process of the information such as coat inside grain morphology clear, crystallite dimension, crystal boundary, and solidification and crystallization form and size distribution ranges by image method quantitatively characterizing plasma spraying YSZ coatings under the cooldown rate being exceedingly fast.This method, which not only deposits different spraying methods different stage ceramic coating micro-structured inner grain form and the characterization of size, has important reference, but also has important theory value to understanding that plasma spraying prepares the formation mechenism of high-performance thermal barrier coating and structure design.
Description
Technical field
The present invention relates to the method clear of thermal barrier coating internal grain form in turbogenerator and large-scale gas turbine.
Background technology
Plasma spraying zirconium dioxide based ceramics thermal barrier coating is widely used in the hot-end component of gas-turbine unit, has
Reduce to effect the heating temperature of matrix.For example, matching somebody with somebody hing straps air film cooling technology, prepared on turbine engine blade surface
The Zirconia Thermal Barrier Coating of 100-500 μ m thicks, can make the surface temperature of Ni/Co based high-temperature alloy matrixes decline 100-
300 DEG C, so as to considerably improve the thermal efficiency of aero-engine, job stability and comprehensive performance.Plasma spraying coating
It is after hitting matrix by a series of molten particles (molten drop), by lateral flow, sprawls, rapid cooling, solidification formation stand piece,
Then stand piece mutually overlaps, stacking forms coating.Therefore, the crystal grain that molten drop is sprawled the solidification stand piece formed and spread out inside piece forms
It is its most basic construction unit.Spread out piece internal grain form, size and spread out interface fine structure between piece, be to influence thermal boundary to apply
The key factor of layer system comprehensive performance.However, grain form and lamella boundary after the solidification of coating microstrueture inner flat
Face, which combines, lacks effectively characterization method clear, this will influence the research of thermal barrier coating microstructure formation mechenism.
At present, transmission electronic microscope technology can to spraying melt drop solidification after grain form, size, crystal structure with
Selecting excellence evaluation is characterized, but since coating sample preparation process is tired of lock, and the microcell of coating can only be characterized, therefore exist
Significant limitation.In contrast, electron backscatter diffraction (EBSD) analytical technology being assemblied in scanning electron microscope
Coat inside crystalline size and shape, crystal boundary, the information such as subgrain and crystal orientation can be obtained, but shortcoming is sample preparation
The stress introduced in journey can influence measurement result.
The content of the invention
It is micro- come plasma spray zirconia (PSZ) base thermal barrier coating clear by thermal etching it is an object of the invention to provide one kind
The technology of institutional framework (grain form) is seen, can farthest disclose the knot after multiple flat solidifications of molten drop inside coating sample
Crystalline form state, has and realizes the characteristics of process is simple, reproducible.
To achieve the above objectives, the present invention, which adopts the following technical scheme that, is achieved：
A kind of method of oxidation zirconium base thermal barrier coating grain form clear, it is characterised in that comprise the following steps：
(1) submicron order YSZ powder materials are used, with plasma spraying method on aluminium alloy base plate, form the oxygen of 2mm thickness
Change zirconium base thermal barrier coating；
(2) alloy matrix aluminum, the metal removal that will be remained on thermal barrier coating are peeled off；Then thermal barrier coating is divided into not
More than 10 × 10mm2Coating test piece；By a wherein surface rubbing and polish, the smooth seamless coating table in surface is formed after cleaning
Face sample；
(3) by coating surface sample in 1250 DEG C, insulation 300min carries out hot etching；
(4) the coating surface sample after being etched to heat is scanned electron microscope observation, and by image method to coating
Surface microstructure is measured and counted；
(5) by step (2) floating coat test piece cutting section, which is polished and polished, coating cross sections are formed after cleaning
Sample, equally in 1250 DEG C, insulation 300min carries out hot etching；
(6) the coating cross sections sample after being etched to heat is scanned electron microscope observation.
In the above method, the coating surface sample preparation is to be sticked to using hot melt adhesive by coating test piece is dispersed
On one circular millstone, mill is placed on autogenous mill downward, coating strip is polished, then with polishing fluid by test piece
Surface polishes, and finally removes polished coating test piece from mill, with ultrasonic cleaner by polished coating test piece
30min is respectively cleaned in acetone and alcohol.
Step (4) described image method is measured and counted to coating surface crystal grain, and wherein described image method refers to take 10
Width amplification factor is 1 × 104, resolution ratio calculates crystallite dimension and counts Grain size distribution for the SEM scanned photographs of 600dpi.
The Grain size distribution uses 11 crystallite dimension sections：<100nm, 100-200nm, 200-300nm ... ...,>1000nm, draws
Crystal grain is in the percentage shared by each section.
It is an advantage of the invention that protected at a certain temperature according to surface of the zirconia-based ceramics coating Jing Guo grinding and polishing light processing
Warm a period of time, since surface energy is different everywhere, grain boundaries atom has the activity of higher, is more easy to by " corrosion ", such crystal grain
The heat etching principle that can be displayed again with crystal boundary, by adjusting heat etching temperature and soaking time, clear its is micro- so as to real
Structure, discloses the crystal habit after multiple flat solidifications of molten drop inside coating sample, measures and count coat inside crystallite dimension
And distribution, draw plasma spraying YSZ coatings in the cooldown rate (10 being exceedingly fast8-109K/s solidification and crystallization form and size under)
Distribution.This result is not only to the ceramic coating micro-structured inner grain form of different spraying methods deposition different stage
And the characterization of size has important reference, and to understanding that plasma spraying prepares the formation mechenism of YSZ thermal barrier coatings
And structure design has important theory value.
Brief description of the drawings
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Fig. 1 is heat etching SEM photograph of the coating sample surface of the present invention when different temperatures insulation 5 is small.Wherein, (a) 800
℃；(b)1100℃；(c)1250℃；(d)1350℃.
Fig. 2 is heat etching SEM photograph of the coating sample surface of the present invention in 1250 DEG C of different soaking times.Wherein, (a)
30min；(b)60min；(c)90min；(d)180min.
Fig. 3 is preferred embodiment of the present invention coating sample surface microstructure statistic figure.Wherein, (a) crystal grain distribution；(b)
Size distribution.
Fig. 4 is present invention contrast SEM photograph.Wherein, (a) non-heat etching coating sample section；(b) when 1250 DEG C of insulations 5 are small
Heat etching coating sample section.
Embodiment
A kind of method of oxidation zirconium base thermal barrier coating internal grain form clear, comprises the following steps：
(1) submicron order YSZ powder materials are used, are sprayed on by plasma spray system on aluminium alloy base plate, are formed
The oxidation zirconium base thermal barrier coating of 2mm thickness；
(2) alloy matrix aluminum is peeled off by wire cutting technology, the metal sand paper remained on thermal barrier coating polishing is gone
Remove；Then thermal barrier coating is divided into the 10 pieces of coating test pieces and numbering painting 1~painting that size is about 10mm × 10mm with glass cutter
10；Then use hot melt adhesive (fusing point for 60-70 DEG C, such as paraffin) wherein to apply 1~apply 8 coating test piece dispersed to be sticked to
On one circular millstone, mill is placed on autogenous mill downward, coating strip is polished, then with polishing fluid by test piece
Surface polishes, and finally removes polished coating test piece from mill, with ultrasonic cleaner by polished coating test piece
30min is respectively cleaned in acetone and alcohol, forms coating surface sample.
(3) 4 (applying 1~painting 4) are taken to be respectively put into 4 corundum earthenwares in the 8 coating surface samples prepared in step (2)
In crucible, be placed in box Muffle furnace respectively with 800 DEG C of different temperatures (applying 1), 1100 DEG C (applying 2), 1250 DEG C (applying 3), 1350 DEG C
(apply 4) carries out hot etching to coating surface, when insulation is 5 small, then carries out displaing microstructure observing by SEM, with reference to figure 1,
It can be seen that from Fig. 1 (c), (d), under 1250 DEG C, 1350 DEG C of heat etching temperature conditionss, effect clear is good, but 1350 DEG C because of temperature
The higher crystal grain that is easy to cause of degree is grown up, therefore the actual selection preferred heat etching temperature of 1250 DEG C of conducts.
(4) the 8 coating surface samples prepared in step (2) are taken into 4 (applying 5~painting 8) still heat more than again
Etching method (is applied with different time 30min (applying 5), 60min (applying 6), 90min (applying 7), 180min respectively under the conditions of 1250 DEG C
8) kept the temperature, displaing microstructure observing is then carried out by SEM, contrasted with reference to figure 2, then with Fig. 1 (c), it is seen that the heat etching time
300min is best；Finally can determine that optimal thermal etching process is 1250 DEG C, keeps the temperature 300min.
Crystallite dimension measurement is carried out to preferred embodiment (applying 3) heat etching sample by image method, (image is that amplification factor is
1×104, resolution ratio 600dpi), take 10 width scanned photographs to calculate and count coated grains Size Distribution.Be divided into [<
100nm], [100-200nm], [200-300nm] ... [>1000nm] 11 crystallite dimension sections, draw crystal grain in each section
Shared percentage.Most of crystal grain distribution can be seen that between 100-400nm by Fig. 3 (a), and in 100-200nm sections institute
It is maximum (32.9%) to account for percentage, as a result with reference to figure 3 (b).This result realizes the quantization of coat inside crystal grain, so as to help
In understanding in microstructure and improve the heat-mechanical performance of ceramic base thermal barrier coating.
Remaining coating test piece " is applied 9 ", " applies 10 " and make coating using the method similar with aforementioned coatings surface sample
Section (perpendicular to surface) sample, wherein " it is right according to the optimal thermal etching process (1250 DEG C, keep the temperature 300min) of step (3) to apply 9 "
Its section carries out heat etching." " applying 10 " samples and carry out microstructure contrast, as a result refer to for 9 " samples and non-heat etching is applied after heat etching
Fig. 4, from Fig. 4 (b) it can be seen that " applying multiple column crystals in 9 " sample layer structures, Coating combination is preferable, against hot-fluid side
It is more consistent to growth, orientation.Confirm the beneficial effect of thermal etching process.
Claims (1)
- A kind of 1. method of oxidation zirconium base thermal barrier coating grain form clear, it is characterised in that comprise the following steps：(1) submicron order YSZ powder materials are used, with plasma spraying method on aluminium alloy base plate, form the zirconium oxide of 2mm thickness Base thermal barrier coating；(2) alloy matrix aluminum, the metal removal that will be remained on thermal barrier coating are peeled off；Then thermal barrier coating is divided into and be not more than 10×10mm2Coating test piece；By a wherein surface rubbing and polish, the smooth seamless coating surface sample in surface is formed after cleaning Product；(3) by coating surface sample in 1250 DEG C, insulation 300min carries out hot etching, and the coating surface sample preparation is to adopt It is sticked to coating test piece is dispersed with hot melt adhesive on a circular millstone, mill is placed on autogenous mill downward, will be applied Layer strip polishes, and then polishes strip with polishing fluid, finally removes polished coating test piece from mill, 30min is respectively cleaned into polished coating test piece in acetone and alcohol with ultrasonic cleaner；(4) the coating surface sample after being etched to heat is scanned electron microscope observation, and by image method to coating surface Crystal grain is measured and counted, and described image method refers to that it is 1 × 10 to take 10 width amplification factors4, resolution ratio is that the SEM of 600dpi is swept Photo is retouched to calculate crystallite dimension and count Grain size distribution, the Grain size distribution uses 11 crystallite dimension sections：<100nm, 100-200nm, 200-300nm ... ...,>1000nm, draws crystal grain in the percentage shared by each section；(5) by step (2) floating coat test piece cutting section, which is polished and polished, coating cross sections sample is formed after cleaning, Equally in 1250 DEG C, insulation 300min carries out hot etching；(6) the coating cross sections sample after being etched to heat is scanned electron microscope observation.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104032255A (en) * | 2014-06-05 | 2014-09-10 | 西安交通大学 | Control method for thermal barrier coating porosity |
| CN104034640A (en) * | 2014-06-05 | 2014-09-10 | 西安交通大学 | Testing method for flattening shape of ceramic molten drops in supersonic speed plasma spraying |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8546284B2 (en) * | 2008-05-07 | 2013-10-01 | Council Of Scientific & Industrial Research | Process for the production of plasma sprayable yttria stabilized zirconia (YSZ) and plasma sprayable YSZ powder produced thereby |
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2015
- 2015-04-07 CN CN201510161679.7A patent/CN104808016B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104032255A (en) * | 2014-06-05 | 2014-09-10 | 西安交通大学 | Control method for thermal barrier coating porosity |
| CN104034640A (en) * | 2014-06-05 | 2014-09-10 | 西安交通大学 | Testing method for flattening shape of ceramic molten drops in supersonic speed plasma spraying |
Non-Patent Citations (1)
| Title |
|---|
| A transmission electron microscopy study of the microstructure and interface of zirconia-based thermal barrier coatings;Y. Wang et al.;《Journal of Alloys and Compounds》;20140916;第619卷;第820页第2栏第2－3段 * |
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