CN105970145A - Preparation method of YSZ thermal barrier coating of sheet micro-nano column crystal structure - Google Patents
Preparation method of YSZ thermal barrier coating of sheet micro-nano column crystal structure Download PDFInfo
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- CN105970145A CN105970145A CN201610332494.2A CN201610332494A CN105970145A CN 105970145 A CN105970145 A CN 105970145A CN 201610332494 A CN201610332494 A CN 201610332494A CN 105970145 A CN105970145 A CN 105970145A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
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- Coating By Spraying Or Casting (AREA)
Abstract
The invention discloses a preparation method of a YSZ thermal barrier coating of a sheet micro-nano column crystal structure. The average thickness of laminated structures (or spreading sheets) formed in different embodiments is measured, so that the thickness of each spreading sheet of the obtained supersonic speed plasma spray coating is approximately one third that of a common plasma spray coating. The structure of the supersonic speed plasma spray coating is represented through a field emission scanning electronic microscope, so that a double-mode microstructure with submicron crystals and nanocrystals coexisting therein appears inside each spreading sheet; and the content of different submicron crystals and nanocrystals inside each spreading sheet is further disclosed through a thermal etching displaying method and a quantitative statistic method.
Description
Technical field
The present invention relates to aero-engine and heavy duty gas turbine turbine blade field, thin particularly to one
The preparation method of sheet micro-nano column crystal structure YSZ thermal barrier coating.
Background technology
Turbo blade is to carry the core component that temperature is the highest, service condition is the harshest in aero-engine.
Even if being single crystal blade material, its carrying temperature extremes also only about 1150 DEG C.Thermal barrier coating is mesh
Before generally acknowledge in the world, the most practicable method of engine blade service temperature can be increased substantially,
Each aviation power is all classified as thermal barrier coating as crucial science and technology.Plasma spraying is to prepare thermal boundary at present to be coated with
A kind of common method of layer.But the most general plasma spraying method, due in plasma jet
Molten drop flight speed is relatively low, and flattening is insufficient, and thickness is relatively to cause coating layer structure (or claiming stand sheet)
Combination rate is low, bond strength is more weak greatly and each other.With the zirconium dioxide that spraying yittrium oxide is partially stabilized
(YSZ), as a example by, great mass of data shows flying of the YSZ molten drop obtained under 9M or the F4 spray gun of import
Line speed is only at about 200m/s, and anchoring strength of coating is generally at below 40MPa.In conjunction with more weak thick
Big stand sheet easily causes coating layering to ftracture under high-temperature hot service condition, causes thermal barrier coating spalling failure,
Therefore must improve existing plasma spray coating process technology, improve molten drop clash into the flight speed before matrix with
Improve the flat ratio of molten drop (between stand sheet area and molten drop green diameter that molten drop is formed after clashing into matrix
Ratio) to obtain the thermal barrier coating that organizational structure is fine and closely woven, high-temperature behavior is excellent, meet China's high-performance boat
Empty electromotor and the needs of heavy duty gas turbine.
Summary of the invention
It is an object of the invention to provide the preparation side of a kind of thin slice micro-nano column crystal structure YSZ thermal barrier coating
Method, has the process of realization simple, reproducible, the feature of remarkable in economical benefits.
For reaching object above, the present invention adopts the following technical scheme that and is achieved:
The preparation method of a kind of thin slice micro-nano column crystal structure YSZ thermal barrier coating, comprises the following steps:
(1) use initial grain size the yittrium oxide of the submicron order of 100-900nm partially stabilized two
Zirconium oxide YSZ particle agglomeration is raw material, and the particle diameter after reunion is 10-50 μm, yittrium oxide matter in raw material
Amount mark is 5% to 8%；
(2) employing has internal powder conveying, prepared by the Supersonic Plasma Spraying method of single anode Laval nozzle
YSZ coating, this coating is used as the ceramic layer in thermal barrier coating system, by spraying coating process in preparation process
Parameter adjustment to following scope, wherein arc current: 300-550A, arc voltage: 115-140V, primary air
Amount: 60-80slpm, secondary air flow: 14-24slpm, spray distance: 80-120mm, powder sending quantity
30-50g/min；
(3) choose the fritter in coating, fritter coating two sides is carried out mechanical reduction and final ion
Thinning, and the most thinning thin district is carried out high resolution transmission electron microscopy observation, obtain coat inside
The thickness of layer structure or stand sheet is 0.61-0.95 μm, obtains micro-nano column crystal structure coating；
(4) remaining coating surface is polished and polishes, after cleaning, form the coating table that smooth surface is seamless
Face sample, by coating surface sample in 1200-1250 DEG C, insulation 180-300min carries out heat erosion.
(5) coating sample after heat erosion is carried out field emission scanning electron microscope observation, and by figure
As coating surface crystal grain is measured and adds up by method, respectively obtain coat inside sub-micron grain and nanometer
The content of crystal grain.
Employing has internal powder conveying, the Supersonic Plasma Spraying method of single anode Laval nozzle prepares YSZ
The substrate temperature of coating controls in the range of 100-200 DEG C.
Described by image method, coating surface crystal grain is measured and adds up refer to that taking 8 width amplifications is 3
×104SEM photograph calculate crystallite dimension and add up 9 crystallite dimension sections < 0.1 μm, 0.1-0.2
μm, 0.2-0.3 μm ..., > percent shared by 0.8 μm.
The technique effect of the present invention:
The present invention is to have internal powder conveying, the Supersonic Plasma Spraying of single anode Laval nozzle by a kind of
Method, under common atmospheric conditions, makes the flight speed of molten drop in plasma jet reach more than velocity of sound,
Thus drastically increase the flat ratio after molten drop clashes into metallic matrix.Simultaneously because contact with metallic matrix
The increase of area, substantially increases the cooldown rate of molten drop, thus is internally formed by nanocrystal at stand sheet
And " thin slice micro-nano cylindrulite " structure that sub-micron grain coexists.On the one hand this structure is favorably improved coating
Structural stability under the high temperature conditions, is on the other hand conducive to improving the thermomechanical property of coating, in boat
Have broad application prospects on empty electromotor and heavy duty gas turbine turbo blade.
Accompanying drawing explanation
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Fig. 1 is the yttrium partially stabilized zirconium dioxide powder body of native oxide that all embodiments of the invention use
Internal grain size.
Fig. 2 is the cross section transmission electron microscopy image that the embodiment of the present invention 1 obtains coating.
Fig. 3 is the cross section transmission electron microscopy image that the present invention contrasts coating sample, and coating uses 9M common
Plasma spraying method obtains.
Fig. 4 is the nanometer crystalline region that the embodiment of the present invention 1 obtains in coating.
Fig. 5 is the submicron crystalline region that the embodiment of the present invention 1 obtains in coating.
Fig. 6 is the microstructure after the embodiment of the present invention 1 obtains coating heat erosion.
Fig. 7 is that the present invention carries out the statistical result of grain size distribution to Fig. 6.
Detailed description of the invention
The preparation method of the present invention a kind of thin slice micro-nano column crystal structure YSZ thermal barrier coating, comprises the steps:
(1) all embodiments are in submicron order (100-900 μm) with crystallite dimension as shown in Figure 1
Partially stabilized zirconium dioxide (YSZ) the reunion powder body of yittrium oxide is spraying raw material, and the particle diameter after reunion is
10-50 μm, in raw material, yittrium oxide mass fraction is 5% to 8%；All embodiments in table 1 all use
Have internal powder conveying, the Supersonic Plasma Spraying method of single anode Laval nozzle prepares YSZ coating.?
In spraying process, the matrix back side uses pressure-air cooling, and temperature controls in the range of 100-200 DEG C.?
In preparation process, spraying parameter is, arc current: 300-550A, arc voltage: 115-140V, main gas
Flow: 60-80slpm, secondary air flow: 14-24slpm, spray distance: 80-120mm, powder feeding
Amount 30-50g/min, concrete technological parameter is as shown in table 1；
(2) choose the fritter in each coating of embodiment 1-20, fritter coating two sides is carried out machinery
It is thinned to the thin slice of 30-60 μ m thick and final ion milling to several nanometers to tens nanometers, and to
The most thinning thin district carries out high resolution transmission electron microscopy observation, obtains coat inside layer structure or stand
The thickness of sheet is 0.61-0.95 μm；
(3) additionally, and choose specific embodiment 1 and compare with common plasma spraying coating, pass through
Graphical analysis obtains the average thickness of the coating layer structure after Supersonic Plasma Spraying or stand sheet and is about
0.71 μm (as shown in Figure 2).The layer structure of the coating of the common plasma spraying of 9M or stand sheet average
Thickness is about 2.10 μm (as shown in Figure 3), and i.e. the former is only the 1/3 of the latter.Coating to embodiment 1
Internal grain form analyzes discovery coat inside further by nanocrystal (as shown in Figure 4) and submicron
Crystal grain (as shown in Figure 5) forms, i.e. the coating of Supersonic Plasma Spraying is a kind of thin slice micro-nano cylindrulite
Structure；
(4) remaining coating is polished at automatic grinding and polishing machine upper surface and polishes, formed after ultrasonic waves for cleaning
The coating surface sample that smooth surface is seamless, by coating surface sample in 1200-1250 DEG C, insulation
180-300min carries out heat erosion；Coating sample after heat erosion is carried out field emission scanning electron microscope
Observe, obtain coat inside and still formed (as shown in Figure 6) by various sizes of crystal grain it was confirmed Supersonic
The double mode microstructure that coating presents nanocrystal and sub-micron grain coexists of speed spraying.By figure
As coating surface crystal grain is measured and adds up by method, choosing 8 width amplifications is 3 × 104SEM shine
Sheet calculates crystallite dimension and adds up 9 crystallite dimension sections (< 0.1 μm, 0.1-0.2 μm, 0.2-0.3
μm ..., > 0.8 μm) shared by percent, find in coating nanocrystal content be about 15% (as
Shown in Fig. 7).
Spraying parameter and the average thickness of coating layer structure under table 1 specific embodiment
Embodiment illustrate the different technical parameters of Supersonic Plasma Spraying coating and coating layer structure or
The average thickness of stand sheet is 0.61-0.95 μm, illustrates that it is a kind of flake structure.
Claims (3)
1. the preparation method of a thin slice micro-nano column crystal structure YSZ thermal barrier coating, it is characterised in that under including
State step:
(1) use initial grain size at the partially stabilized dioxy of the yittrium oxide of the submicron order of 100-900nm
Changing zirconium YSZ particle agglomeration is raw material, and the particle diameter after reunion is 10-50 μm, and in raw material, yittrium oxide quality is divided
Number is 5% to 8%；
(2) employing has internal powder conveying, the Supersonic Plasma Spraying method of single anode Laval nozzle prepares YSZ
Coating, this coating is used as the ceramic layer in thermal barrier coating system, is adjusted by spraying parameter in preparation process
To following scope, wherein arc current: 300-550A, arc voltage: 115-140V, primary air amount: 60-80slpm,
Secondary air flow: 14-24slpm, spray distance: 80-120mm, powder sending quantity 30-50g/min；
(3) choose the fritter in coating, fritter coating two sides is carried out mechanical reduction and final ion subtracts
Thin, and the most thinning thin district is carried out high resolution transmission electron microscopy observation, obtain coat inside stratiform knot
The thickness of structure or stand sheet is 0.61-0.95 μm, obtains micro-nano column crystal structure coating；
(4) remaining coating surface is polished and polishes, after cleaning, form the coating surface that smooth surface is seamless
Sample, by coating surface sample in 1200-1250 DEG C, insulation 180-300min carries out heat erosion；
(5) coating sample after heat erosion is carried out field emission scanning electron microscope observation, and pass through image
Coating surface crystal grain is measured and adds up by method, respectively obtains coat inside sub-micron grain and nanocrystal
Content.
The preparation method of a kind of thin slice micro-nano column crystal structure YSZ thermal barrier coating the most according to claim 1,
It is characterized in that, employing has internal powder conveying, prepared by the Supersonic Plasma Spraying method of single anode Laval nozzle
The substrate temperature of YSZ coating controls in the range of 100-200 DEG C.
The preparation method of a kind of thin slice micro-nano column crystal structure YSZ thermal barrier coating the most according to claim 1,
It is characterized in that, described by image method, coating surface crystal grain is measured and adds up refer to take 8 width times magnifications
Number is 3 × 104SEM photograph calculate crystallite dimension and add up 9 crystallite dimension sections < 0.1 μm, 0.1-0.2
μm, 0.2-0.3 μm ..., > percent shared by 0.8 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109457211A (en) * | 2018-12-21 | 2019-03-12 | 西安交通大学 | A kind of wear resistant friction reducing coating production of lubrication phase highly dispersed distribution |
| CN109628872A (en) * | 2018-12-20 | 2019-04-16 | 西安交通大学 | The stable thin slice micro-nano column crystal structure YSZ method for preparing heat barrier coating of phase constituent |
| CN115044852A (en) * | 2022-05-12 | 2022-09-13 | 西安交通大学 | Nanoscale column/hole/amorphous structure thermal barrier coating and preparation method thereof |
Citations (3)
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|---|---|---|---|---|
| CN102963061A (en) * | 2012-12-03 | 2013-03-13 | 上海理工大学 | Nano columnar crystal thermal barrier coating layer and preparation method thereof |
| CN103009704A (en) * | 2011-09-21 | 2013-04-03 | 中国农业机械化科学研究院 | Nanometer/columnar-like crystal mixing structure thermal barrier coating and preparation method thereof |
| WO2013085625A2 (en) * | 2011-10-17 | 2013-06-13 | Directed Vapor Technologies International | Impact and erosion resistant thermal and environmental barrier coatings |
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2016
- 2016-05-18 CN CN201610332494.2A patent/CN105970145A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103009704A (en) * | 2011-09-21 | 2013-04-03 | 中国农业机械化科学研究院 | Nanometer/columnar-like crystal mixing structure thermal barrier coating and preparation method thereof |
| WO2013085625A2 (en) * | 2011-10-17 | 2013-06-13 | Directed Vapor Technologies International | Impact and erosion resistant thermal and environmental barrier coatings |
| CN102963061A (en) * | 2012-12-03 | 2013-03-13 | 上海理工大学 | Nano columnar crystal thermal barrier coating layer and preparation method thereof |
Non-Patent Citations (1)
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| 韩志海 等: "超音速等离子喷涂制备细密柱晶结构热障涂层研究进展", 《热喷涂技术》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109628872A (en) * | 2018-12-20 | 2019-04-16 | 西安交通大学 | The stable thin slice micro-nano column crystal structure YSZ method for preparing heat barrier coating of phase constituent |
| CN109457211A (en) * | 2018-12-21 | 2019-03-12 | 西安交通大学 | A kind of wear resistant friction reducing coating production of lubrication phase highly dispersed distribution |
| CN115044852A (en) * | 2022-05-12 | 2022-09-13 | 西安交通大学 | Nanoscale column/hole/amorphous structure thermal barrier coating and preparation method thereof |
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