CN103710662A - Oxide thermal barrier coating with micron/nanometer equiaxed crystal structure and preparation method for oxide thermal barrier coating - Google Patents
Oxide thermal barrier coating with micron/nanometer equiaxed crystal structure and preparation method for oxide thermal barrier coating Download PDFInfo
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- CN103710662A CN103710662A CN201310712301.2A CN201310712301A CN103710662A CN 103710662 A CN103710662 A CN 103710662A CN 201310712301 A CN201310712301 A CN 201310712301A CN 103710662 A CN103710662 A CN 103710662A
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Abstract
The invention discloses an oxide thermal barrier coating with a micron/nanometer equiaxed crystal structure and a preparation method for the oxide thermal barrier coating. The thermal barrier coating consists of oxide, has the equiaxed crystal structure and an equiaxed crystal rate of more than or equal to 90 percent, comprises more than 80 percent of equiaxed crystal grains with sizes of 500nm, and is prepared by spray-coating agglomerated powder on the surface of a metal substrate in an ultra-low pressure plasma spray-coating way. A coating with a completely nanometer equiaxed crystal structure can be prepared under proper process conditions. The coating is structurally different from a conventional thermal barrier coating which is formed by a plasma spray-coating mode and contains a few nanometer structures, has the characteristics of low thermal conductivity, high thermal shock resistance and the like, and can be widely applied.
Description
Technical field
The present invention relates to preparation technology of coating, relate in particular to the thermal barrier coating that is applied to the high temperature metal part surfaces such as aircraft engine, belong to thermospray Surface-micromachining process.
Background technology
Thermal barrier coating has been widely used in high-temperature turbine engine parts, aircraft engine combustion chamber for example, and the high-temperature alloy surfaces such as turbine blade and stationary guide blades, to reducing high-temperature alloy surface temperature, improve motor efficiency and play an important role.Thermal barrier coating, mainly by the anti-oxidant matrix metal layer of high-temperature alloy surface with have low heat conductivity, form compared with the ceramic coating of high expansion coefficient, the present invention relates to a kind of preparation method with the heat insulating ceramic coat of micro-or nano size equiax crystal structure.
Up to the present, the weave construction of the heat insulating ceramic coat of exemplary practical mainly contains two kinds, and the one, air plasma spraying forms with the stratiform of gapped pore piles up tissue; Another kind be electro beam physics vapour deposition prepare there is the coating perpendicular to matrix surface independence columnar crystal structure.Yet the equal defectiveness of the coating of these two kinds of different structures, sheet is piled up coating and is had the low (0.8～1.2Wm of thermal conductivity
-1k
-1) advantage, but resistance to heat shocks is poor, and the life-span is short, may come off, so this type coating only limits to apply inessential piece surface in use.Although column crystal coating heat-shock resistance is better, the high (1.5～2.0Wm of thermal conductivity of this structure coating
-1k
-1), effect of heat insulation is bad, and preparation cost is high.In order to improve heat-shock resistance and the thermal conductivity of thermal barrier coating, plasma spraying nano particle is prepared coating becomes study hotspot, comprising liquid material spraying method, and United States Patent (USP) (application number: 20130095340A1) for example.Fig. 1 is that nano particle forms coating schematic diagram, the problem that atmospheric plasma spraying agglomerated nanocrystalline powder faces is, easily fusing completely of nano particle in spraying process, be combined into larger micron particle, as shown in number in the figure 1, under plasma jet guiding, striking work surface, produce collision and flatten into traditional lamellar structure, only have a small amount of semi-molten or do not melt nano particle to be kept in coating.As shown in number in the figure 2 and 3, the final coating structure nanometer primary particle forming keeps seldom, as shown in Figure 2.Therefore, how improving the ratio of nano particle in coating is the direction that investigator makes great efforts.
The U.S. 7,413,798 patents propose to sneak into nanometer column crystal in laminate structure and alleviate coating high-temp-cooling stress concentration; United States Patent (USP) 8,147,928 and 6,548,190 have proposed to sneak into other material to yttria-stabilized zirconia coating, reduce the method for column crystal coating thermal conductivity.These patents all belong to the improvement research of carrying out on existing coating basis above, different from the high thermal barrier coating of nanometer equiax crystal of the present invention.Domestic patent (application number: 200710118139) propose a kind of ceramic heat-barrier coating of stabilizing zirconium oxide by Yttrium oxide preparation technology and material and production method.This thermal barrier coating has novel nano particle and the common composite structure forming of honeycomb-like network.Domestic patent (application number: 200510019464) also propose a kind of method that liquid phase plasma spraying is prepared nanometer zirconia heat barrier coating.From actual coating, liquid phase plasma spraying coating particles bonding strength is low, is different from nanometer equiax crystal ceramic coating of the present invention.
To sum up related patent is all different from the oxide compound thermal barrier coating patent with micro-/ nano equiaxed grain structure that the present invention proposes.
Summary of the invention
For solving in Plasma Spraying Process Using, the easy melted join of nano particle becomes larger micron particle, thereby be difficult to obtain the equiax crystal structure of nano-scale, and existing coating thermal conductivity is high, resistance to heat shocks is poor, the problem that the life-span is short, the invention provides a kind of thermal barrier coating with micro-/ nano equiaxed grain structure, thermal barrier coating of the present invention has the equiax crystal structure of micro/nano level, and thermal conductivity is low, and resistance to sudden heating is strong.Technical purpose of the present invention is achieved through the following technical solutions:
An oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure, by being selected from Gd
2o
3, Yb
2o
3, Nd
2o
3, Er
2o
3, La
2o
3or Y
2o
3in one or more and ZrO
2the composite oxides that form form, and it is characterized in that described thermal barrier coating is equiax crystal structure, equiaxial crystal ratio>=90%, and equi-axed crystal is of a size of 30nm～2 μ m, and wherein equi-axed crystal size < 500nm's accounts for more than 80%.
Equiaxial crystal ratio of the present invention has following implication: the shared ratio of equiax crystal area in coating unit area; Described equi-axed crystal size refers to the mean value of the component units-single Polygons crystal grain all directions diameter of equiax crystal structure.
The oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure of the present invention, as preferably, described composite oxides are yttrium oxide PSZ, are ZrO
2-(6-8) wt%Y
2o
3.
Yttrium oxide PSZ is the most frequently used ceramic heat-barrier coating, but this material high-temperature service process, and due to the high temperature sintering of material, grain-size, hardness, Young's modulus that makes thermal barrier coating etc. changes.To take zirconium white, in main material, add some rare earth oxides, as Gd for this reason
2o
3, Yb
2o
3, Nd
2o
3, Er
2o
3, La
2o
3have and suppress take the effect of zirconium white as main thermal barrier coating grain growing and coating performance variation.But the action effect of every kind of rare earth oxide is not quite similar, its addition is still one of research direction of this area.In technical scheme of the present invention, in conjunction with the common practise of this area, have reason to believe Gd
2o
3, Yb
2o
3, Nd
2o
3, Er
2o
3, La
2o
3deng rare earth oxide and ZrO
2composite oxides also can reach technique effect of the present invention.
The oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure of the present invention, when equiaxial crystal ratio < 100%, the non-equiax crystal structure of take exists particle as columnar crystal structure.
Further, as most preferred technical scheme, the equiaxial crystal ratio with the oxide compound thermal barrier coating of micro-/ nano equiaxed grain structure of the present invention is 100%.
The preparation method that the oxide compound thermal barrier coating of micro-/ nano equiaxed grain structure is provided described in another technical purpose of the present invention is to provide, adopts ultralow pressure plasma spraying method that the reunion powder of the described composite oxides of 30～80 μ m is sprayed on to metal substrate surface;
The parameter of described ultralow pressure plasma spraying is: environmental stress is 50～1000Pa, and flame current is 400～1200 amperes, and arc voltage is higher than 30 volts, and powder sending quantity is 3～30 gram/minute, and spray distance is 200～600 millimeters.
In preparation method of the present invention, when spraying, according to different objects, can select to be sprayed into different substrate surfaces, as the surface of metal parts, superalloy or hot metal tack coat.
The preparation method with the oxide compound thermal barrier coating of micro-/ nano equiaxed grain structure of the present invention, as technical scheme more preferably, the parameter of described ultralow pressure plasma spraying is: environmental stress is 50～500Pa, flame current is 500～1000 amperes, arc voltage is higher than 30 volts, powder sending quantity is 3～20 gram/minute, and spray distance is 300～600 millimeters.
Further, as most preferred technical scheme, the parameter of described ultralow pressure plasma spraying is:
Ultralow pressure plasma spraying of the present invention, plasma working gas used is: Ar/H
2/ He=(40-50)/(5-15)/(10-30) liter/min, powder feeding carrier is: Ar3-5 liter/min.
The preparation method with the oxide compound thermal barrier coating of micro-/ nano equiaxed grain structure of the present invention, the interior porosity of the reunion powder of preferred described composite oxides is 10～50%.
The preparation method with the oxide compound thermal barrier coating of micro-/ nano equiaxed grain structure of the present invention, the nano-oxide particles that the reunion powder of preferred described composite oxides is 20～300nm by particle diameter is reunited and is formed.The size of selected original nano-oxide directly affects the size of equiax crystal particle size in the coating after spraying.
In preparation method of the present invention, the reunion powder preparation method of described composite oxides is more, includes but are not limited to following methods:
Mixing-agglomeration process: such as methods such as spraying are dried.
Sintering-crush method: the powder that contains nano material is added to agglutinant, sinter massive material under proper temperature, be then broken into micron particles; Or nano powder is mixed with nanometer BN and organic gel, adjust mixture ratio, high temperature sintering, now BN becomes steam and is burnt, and leaves pore, and nanometer blocks after sintering is broken into a micron powder;
It is as follows that wherein spray drying process is prepared the concrete operation step of described reunion powder:
The nano-oxide particles that is 20～300nm by particle diameter and polyvinyl alcohol caking agent are by (80～90): the mass ratio of (5～10) mixes, add again the water of 1.0～1.5 times of quality to be deployed into slurry, adopt spraying to be dried within the scope of 280～300 ℃ and make reunion powder, reunion powder is placed in to sintering oven sintering, improve reunion powder intensity, sintering temperature is 800～1200 ℃.
Beneficial effect of the present invention:
1. the present invention adopts thermal barrier coating prepared by ultralow pressure plasma spraying method, there is micro-/ nano equiax crystal structure, equiaxial crystal ratio reaches more than 90%, and equi-axed crystal size < 500nm accounts for more than 80%, under the experiment condition of optimizing, even can obtain equiaxial crystal ratio and be 100% complete equiax crystal structure, this is the result not reached in ceramic heat-barrier coating research before, the equiax crystal structure of micro/nano level has been improved the character of coating to a great extent, thermal barrier coating heat shock resistance power of the present invention is good, thermal conductivity is low, Application Areas is more extensive,
2. thermal barrier coating of the present invention can be used for the thermal insulation protection of the metalworks such as aircraft engine high temperature blade, combustion chamber, also can be used for high temperature seal coating;
3. the coating performance that prepared by the present invention is good, and cost is low.
Accompanying drawing explanation
Accompanying drawing 7 width of the present invention,
Fig. 1. current plasma spraying nano-structured coating schematic diagram, wherein 1-melts particle completely, 2-semi-molten particle, 3-other nano particle tissue, 4-melts solidifying of particle completely, 5-pore;
Fig. 2. current plasma spraying nano-structured coating Electronic Speculum figure;
The electron-microscope scanning figure of the composite oxides reunion powder individual particle that Fig. 3 .(a) prepared by the present invention; (b) the composite oxides reunion powder particle surface enlarged view that prepared by the present invention;
Fig. 4. the one-piece construction Electronic Speculum figure of thermal barrier coating prepared by the present invention;
Fig. 5. the amplification Electronic Speculum figure in thermal barrier coating cross section prepared by the present invention;
Fig. 6. the thermal conductivity of thermal barrier coating prepared by the present invention and the comparison of other coating;
Fig. 7. the thermal-shock resistance picture of thermal barrier coating prepared by the present invention, wherein (a) and (b) be respectively experiment before and after picture.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
1. the preparation of oxide agglomerate powder:
The yttrium oxide PSZ powder ZrO that purchase granularity is 80～180nm
2-(7-8) wt%Y
2o
3, mix by the mass ratio of 90:10 with polyvinyl alcohol caking agent, add again 1.5 times to the water purification of mixture weight, be deployed into slip, adopt spraying dry, by controlling drying temperature, control the void content of reunion powder, controlling spraying drying temperature is 280～300 ℃, make micron order reunion powder, powder is placed in to sintering oven sintering, improve reunion powder intensity, sintering temperature is 800 ℃, utilize scanning electron microscope and laser particle analyzer to carry out porosity and aggregation size sign to agglomerated nanocrystalline powder, described reunion powder particle diameter is 35～80 microns, porosity is 25～40%, confirm to meet requirement of the present invention.As shown in Figure 3, be (a) the electron-microscope scanning figure of the composite oxides reunion powder individual particle of preparation, (b) be composite oxides reunion powder particle surface enlarged view.
2. ultralow pressure Thermal Barrier Coating Layers Prepared By Plasma Spraying
Adopt the low pressure plasma spray gun (having obtained national inventing patent ZL201010288490.1) of Dalian Maritime University's development, in low pressure vessel, implement spraying, set spray parameters as follows:
According to the parameter of above-mentioned setting, the ZrO at FeCrAl high-temperature alloy surface being prepared by step 1
2-(7-8) wt%Y
2o
3reunion powder, adopts ultralow pressure plasma spraying to prepare the exemplar that coat-thickness is 0.3mm.Thermal barrier coating prepared by the present invention, during spraying yttrium oxide PSZ, needing ultralow-voltage plasma spraying equipment, the environmental stress of spraying is 50-1000Pa, far below the pressure 5000-8000Pa of traditional low-voltage plasma spraying.There are the companies such as Sulzer Metco in the external manufacturer of ultralow-voltage plasma spraying equipment.Ultralow-voltage plasma spraying equipment of the present invention is the equipment of Dalian Maritime University's development.
3. sample evaluation
1. equiax crystal structure: adopt sweep electron microscopic measure equiaxial crystal ratio to reach 100%, and the ratio of equi-axed crystal size below 500nm reaches more than 80%, be illustrated in figure 4 the one-piece construction Electronic Speculum figure of the thermal barrier coating of preparation, Fig. 5 is the amplification Electronic Speculum figure in thermal barrier coating cross section.
2. thermal conductivity: laser heating method, the thermal conductivity of having measured thermal barrier coating prepared by the present invention in 300～450 ℃ of scopes of temperature is 0.55～0.7Wm
-1k
-1, as a comparison, as a comparison, the thermal conductivity of thermal barrier coating of the present invention is lower than traditional plasma-sprayed coating layers sheet coating level (1.2～1.4m for traditional plasma-sprayed coating layers sheet coating and air plasma spraying large size equiax crystal coating
-1k
-1) and air plasma spraying large size equiax crystal coating (0.8～0.9m
-1k
-1), as shown in Figure 6, coating thermal conductivity advantage of the present invention is very obvious.
Wherein the spray parameters of traditional plasma-sprayed coating layers sheet coating is: electric current 650A, voltage 60V, broken powder, powder feeding rate 20 gram/minute, spray distance 100mm.
The spray parameters of air plasma spraying large size equiax crystal coating is: electric current 400A, voltage 55V, agglomeration nano powder, powder feeding rate 15 gram/minute, spray distance 100mm.
3. heat-cold shock destructive test: the exemplar of coating is heated to 1100 ℃, keeps 10 minutes, adopt high-pressure air (0.4MPa) to be cooled to nearly room temperature, repeated multiple times operation.Through heating-cooling 1000 thermal cyclings, coating is substantially intact.In Fig. 7 (a) and (b) be respectively the comparison of sample before and after experiment, show that nanometer equiax crystal coating prepared by the present invention has good resistance to sudden heating.
By above experimental result, can be reached a conclusion: thermal barrier coating of the present invention has micro-/ nano equiax crystal structure, and equiaxial crystal ratio reaches 100%, the ratio of equi-axed crystal size below 500nm reaches more than 80%; Coating thermal conductivity is low, and cold-hot impact is good, therefore has application widely.
Claims (6)
1. an oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure, by being selected from Gd
2o
3, Yb
2o
3, Nd
2o
3, Er
2o
3, La
2o
3or Y
2o
3in one or more and ZrO
2the composite oxides that form form, and it is characterized in that described thermal barrier coating is equiax crystal structure, equiaxial crystal ratio>=90%, and equi-axed crystal is of a size of 30nm～2 μ m, and wherein equi-axed crystal size < 500nm's accounts for more than 80%.
2. the oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure according to claim 1, is characterized in that in the equiax crystal structure of described thermal barrier coating, equiaxial crystal ratio is 100%.
3. the oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure according to claim 1, is characterized in that described composite oxides are yttrium oxide PSZ.
4. the oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure described in claim 1～3 any one, is characterized in that adopting ultralow pressure plasma spraying method that the reunion powder of the described composite oxides of 30～80 μ m is sprayed on to metal substrate surface;
The parameter of described ultralow pressure plasma spraying is: environmental stress is 50～1000Pa, and flame current is 400～1200 amperes, and arc voltage is higher than 30 volts, and powder sending quantity is 3～30 gram/minute, and spray distance is 200～600 millimeters.
5. the oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure according to claim 4, the interior porosity that it is characterized in that the reunion powder of described composite oxides is 10～50%.
6. the oxide compound thermal barrier coating with micro-/ nano equiaxed grain structure according to claim 4, the nano-oxide particles that the reunion powder that it is characterized in that described composite oxides is 20～300nm by particle diameter is reunited and is formed.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107012420A (en) * | 2017-04-06 | 2017-08-04 | 江西省科学院应用物理研究所 | A kind of method that plasma spraying technology prepares erbium oxide tritium permeation barrier |
| CN113087521A (en) * | 2019-12-23 | 2021-07-09 | 中国科学院上海硅酸盐研究所 | Preparation method of thermal barrier coating with controllable crystal morphology |
| CN114101704A (en) * | 2021-11-23 | 2022-03-01 | 中北大学 | High-strength TC4-BN alloy containing equiaxed crystal and columnar crystal mixed structure and preparation method thereof |
| CN117551365A (en) * | 2024-01-10 | 2024-02-13 | 北矿新材科技有限公司 | Powder for sealing coating, sealing coating and preparation method of sealing coating |
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2013
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Patent Citations (2)
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| JPH0769796A (en) * | 1993-06-30 | 1995-03-14 | Kokusai Chodendo Sangyo Gijutsu Kenkyu Center | Method for forming film of oxide on metal substrate by heraty plasma evaporation method |
| EP1666437A2 (en) * | 2004-12-06 | 2006-06-07 | General Electric Company | Sintering resistant, low thermal conductivity, high stability thermal barrier coating/environmental barrier coating system for a silicon containing substrate to improve high temperature capability |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107012420A (en) * | 2017-04-06 | 2017-08-04 | 江西省科学院应用物理研究所 | A kind of method that plasma spraying technology prepares erbium oxide tritium permeation barrier |
| CN113087521A (en) * | 2019-12-23 | 2021-07-09 | 中国科学院上海硅酸盐研究所 | Preparation method of thermal barrier coating with controllable crystal morphology |
| CN114101704A (en) * | 2021-11-23 | 2022-03-01 | 中北大学 | High-strength TC4-BN alloy containing equiaxed crystal and columnar crystal mixed structure and preparation method thereof |
| CN114101704B (en) * | 2021-11-23 | 2023-11-28 | 中北大学 | High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof |
| CN117551365A (en) * | 2024-01-10 | 2024-02-13 | 北矿新材科技有限公司 | Powder for sealing coating, sealing coating and preparation method of sealing coating |
| CN117551365B (en) * | 2024-01-10 | 2024-04-16 | 北矿新材科技有限公司 | Powder for sealing coating, sealing coating and preparation method of sealing coating |
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Application publication date: 20140409 |