US20190292645A1 - Self-healing heat damping layers and method for producing same - Google Patents

Self-healing heat damping layers and method for producing same Download PDF

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Publication number
US20190292645A1
US20190292645A1 US16/301,445 US201716301445A US2019292645A1 US 20190292645 A1 US20190292645 A1 US 20190292645A1 US 201716301445 A US201716301445 A US 201716301445A US 2019292645 A1 US2019292645 A1 US 2019292645A1
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heat
powder
mosi
layer
insulating layer
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Robert Vassen
Denise Koch
Karl-Heinz Rauwald
Wim G. Sloof
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Forschungszentrum Juelich GmbH
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Forschungszentrum Juelich GmbH
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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
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • 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
    • 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

Definitions

  • the invention relates to of high-temperature barrier coatings, and in particular, to ceramic heat-insulating layers (HIL), as used in gas turbines or aircraft turbines.
  • HIL ceramic heat-insulating layers
  • Starting materials for high-temperature substrates in an oxidizing environment are generally those which continuously form a thermodynamically stable oxide layer. This oxide layer acts as a barrier between the environment and the high-temperature substrate itself.
  • Alloys that have proven to be particularly suitable are inter alia those that form an aluminum oxide (Al 2 O 3 ), a silicon dioxide (SiO 2 ) or a chromium oxide (Cr 2 O 3 ) layer.
  • Al 2 O 3 aluminum oxide
  • SiO 2 silicon dioxide
  • Cr 2 O 3 chromium oxide
  • the high-temperature substrates are first provided with a diffusion barrier coating as an adhesion-promoter layer, on which an additional thermal barrier coating (TBC) is generally arranged as the uppermost layer.
  • TBC thermal barrier coating
  • heat-insulating layer such as gadolinium zirconate or zirconia together with additional stabilizing components such as MgO, CaO or CeO 2 .
  • cracks may develop in the heat-insulating layer due to the thermal load, since YSZ can undergo a phase change at high temperatures.
  • cracks often occur in the heat-insulating layer due to oxidation of the adhesion-promoter layer.
  • Derelioglu et al. [4] selected a solution in which boron-doped MoSi 2 was used as a sacrificial material in a YSZ heat-insulating layer, and this was intended to automatically heal thermally induced cracks.
  • enclosed MoSi 2 (B) particles adjacent to cracks are preferably intended to oxidize and in the process form an amorphous SiO 2 phase, which penetrates into the developing cracks and fills and closes said cracks again by forming solid ZrSiO 4 .
  • the success of the self-healing heat-insulating layer depends heavily on the size of the MoSi 2 (B) particles introduced and the distribution thereof.
  • MoSi 2 is very susceptible to oxidation.
  • Sloof et al. [5] proposed that these should be enclosed in a protective coating that provides protection against oxidation but also allows crack formation due to this protective coating and in this case also permits the MoSi 2 to oxidize.
  • ⁇ -Aluminum oxide ( ⁇ -Al2O3), zirconium (ZrSiO4) and mullite (Al 6 Si 2 O 13 ) are mentioned as particularly suitable materials for this type of barrier coating and are preferably applied to the MoSi 2 particles by means of a sol-gel method or atomic layer deposition (ALD).
  • the present invention provides a method for producing a self-healing heat-insulating layer on a substrate by atmospheric plasma spraying (APS) of a heat-insulating-layer powder.
  • the method includes introducing MoSi2 powder containing aluminum into a heat-insulating layer.
  • the MoSi2 powder contains aluminum in a content of from 2 to 15 wt. %.
  • the MoSi2 powder is used in a mass fraction of between 0.5 and 5 wt. % based on the heat-insulating layer.
  • the method further includes injecting the heat-insulating-layer powder at a first point that is at a distance from a gun in the axial direction and injecting the MoSi2 powder into a plasma jet at a second point that is at a greater distance from the gun in the axial direction.
  • An injection distance (I) of between 20 and 60 mm is set between the first and the second point.
  • FIG. 1 shows the double-injection principle, as used in the method according to the invention
  • Embodiments of the invention provide systems and methods for healing cracks that develop in a ceramic heat-insulating layer during operation of a component to be protected and thus prevent premature flaking off of the heat-insulating layer.
  • Embodiments of the invention provide new and improved self-healing heat-insulating layers which have the above-mentioned features and which are suitable for use in high-temperature processes involving thermal cycling. Furthermore, embodiments of the invention provide corresponding production methods for such self-healing heat-insulating layers.
  • a heat-insulating layer in particular a zirconium-containing heat-insulating layer
  • the self-healing properties of a heat-insulating layer can be significantly improved by introducing MoSi 2 , by certain conditions being maintained during the production of the heat-insulating layer.
  • Y 2 O 3 -stabilized zirconia is in particular considered to be a heat-insulating-layer material suitable therefor.
  • MgO-, Cao- or CeO 2 -stabilized zirconia are also suitable as a heat-insulating-layer material therefor.
  • other oxides such as MgAl 2 O 4 , Al 2 O 3 , TiO 2 , mullite, La 2 Zr 2 O 7 or Gd 2 Zr 2 O 7 , or also Y—Si—O compounds, can be used as suitable heat-insulating-layer materials within the meaning of this invention.
  • MoSi 2 powder containing aluminum can be used.
  • the approach of in situ coating can be selected for coating the self-healing MoSi 2 particles with aluminum oxide.
  • the corresponding MoSi 2 particles, which additionally contain aluminum are first integrated in the heat-insulating layer by means of atmospheric plasma spraying (APS).
  • a protective Al 2 O 3 coating is then formed around the MoSi 2 particles by means of heat treatment in situ. This requires a sufficient aluminum reservoir to be contained in the MoSi 2 particles.
  • the MoSi 2 powder used therefore contains aluminum in a mass fraction of from 2 to 15 wt. %, preferably in a mass fraction of between 3 and 12 wt. %.
  • the MoSi 2 powder used may also contain boron in a maximum mass fraction of up to 2 wt. %.
  • the MoSi 2 powder is only added to the heat-insulating layer up to a maximum proportion of 5 wt. % of the heat-insulating layer.
  • the MoSi 2 powder is used in a proportion of between 0.1 and 5 wt. % based on the heat-insulating layer.
  • the service life of the heat-insulating layers can be significantly increased in comparison with the YSZ layers used as standard.
  • the cracks are filled within the zirconium-containing heat-insulating layer by the oxidation of MoSi 2 , as a result of which SiO 2 is formed.
  • MoSi 2 oxidation of MoSi 2
  • This is generally in a glass-like phase, meaning that even long cracks can be filled.
  • the MoO 3 that is likewise formed is in the gas phase within the operating temperature and evaporates accordingly.
  • the SiO 2 formed can react with the ZrO 2 in the heat-insulating layer and form zirconium (ZrSiO 4 ). Owing to this reaction, cracks are prevented from re-forming at the same point, since the reaction means that there is no longer a clear boundary between the two materials which could be a weak point. The developing cracks are accordingly healed by the developing SiO 2 and the subsequent reaction with the ZrSiO 4 .
  • the temperature of the MoSi 2 powder introduced is another significant point in the production of a self-healing heat-insulating layer according to embodiments of the invention.
  • the heat-insulating layer is produced by means of atmospheric plasma spraying (APS) and that a second, separate injection point for supplying the MoSi 2 powder is selected in addition to the supply of the heat-insulating-layer powder itself.
  • This second injection point is advantageous in that MoSi 2 can be prevented from breaking down during application and, at the same time, the heat-insulating-layer powder is optimally utilized as the matrix material for the heat-insulating layer.
  • the MoSi 2 coating requires relatively low plasma-gas temperatures in order to prevent the material breaking down.
  • the plasma gas needs to have sufficient energy to melt the heat-insulating-layer powder, e.g. YSZ, if homogeneous mixed layers made of both materials are to be produced.
  • a special injection method (double-injection system) is therefore proposed, as shown schematically in FIG. 1 , in which the MoSi 2 powder and YSZ powder are separately injected as the heat-insulating-layer powder.
  • the supply point for the MoSi 2 powder is at a second point that is at a distance from the gun in the axial direction.
  • a special injection holder is provided for this purpose.
  • the injection distance between the supply of YSZ and MoSi 2 (I) and the injection depth in relation to the plasma-jet axis (d) can be set as desired on the APS equipment.
  • the temperature of the plasma decreases from the plasma source towards the substrate to be coated.
  • the plasma thus consistently has a higher temperature at the point of supply of the heat-insulating-layer powder than at the point of supply of the MoSi 2 powder.
  • tests using the plasma gas (Ar:He) together with different currents and a total spraying distance of approx. 120 mm to the surface of the substrate were carried out in particular.
  • the injection distance was varied between 20 and 50 mm in this case.
  • a significant increase in the service life of the thus produced heat-insulating layer was demonstrated for selected injection distances of above 30 mm in particular.
  • the layer thickness per spraying pass is generally reduced as the current decreases, since a lower current generates a plasma that has less energy. As a result, fewer completely molten particles are formed, which leads to reduced layer deposition.
  • the spraying distance also needs to be consistently increased in order to achieve the same effect, in particular the porosity to be achieved.
  • the injection distance should also be increased. If the injection distance is increased, finer particles can be used, the current can be increased and the quantity of the conveying gas for the MoSi 2 powder can also be increased. If the spraying distance is increased, the current should be accordingly increased.
  • the particles supplied to the plasma generally have more time to melt before they reach the surface of the substrate.
  • the injection distance (I) it is ensured according to the invention that there is only a low spraying distance for the MoSi 2 powder supplied, and this therefore also reduces the length of time that the MoSi 2 particles remain in the plasma-gas jet. This ensures that the supplied MoSi 2 particles do melt, but the material does not break down, while at the same time the spraying distance is enough to sufficiently melt the supplied heat-insulating-layer powder.
  • the spraying distance and the selected current also have an effect on the porosity of the deposited layer, in combination with the powder used.
  • the injection distance should be reduced and/or the current should be accordingly increased.
  • the selection of the plasma gas for example (Ar:He), (Ar:H 2 ) or (Ar:N 2 ), has a significant impact on the parameters to be set, since different temperatures are generated depending on the plasma gas, i.e. a change in the plasma composition consistently leads to a change in the temperature and speed.
  • a current of at least 400 A is suggested, preferably of 420 or 470 A. This does also depend on the gun that is used, however.
  • the current can therefore be increased and/or the injection distance can be decreased.
  • the current should be decreased and/or the injection distance should be increased.
  • the parameters of the conveying gas for the MoSi 2 powder e.g. the distance from the plasma axis (d) or the quantity or speed of the conveying gas, should be selected such that the MoSi 2 powder supplied is injected centrally into the plasma jet.
  • the depth of the injection relative to the plasma-jet axis for the MoSi 2 powder has an effect in this respect, since turbulence often occurs at the edges of the plasma jet.
  • MoSi 2 powder is used with an average particle diameter (d 50 ) of between 5 and 60 ⁇ m, preferably with an average particle diameter (d 50 ) of between 10 and 50 ⁇ m.
  • porous heat-insulating layers are deposited which have the same or slightly increased porosity in comparison with standard heat-insulating layers that are conventionally deposited by means of APS.
  • the porosities of standard YSZ heat-insulating layers deposited by means of APS are consistently between 15 and 25 vol. % in this case.
  • the open porosity of the heat-insulating layers deposited according to the invention was determined in this case by means of image analysis of images of cut layers, and is between 17 and 20 vol. %.
  • thermocycling involves a 2-hour high-temperature phase at approx. 1100° C. followed by a 15-minute low-temperature phase at approx. 60° C.
  • the chemical composition of the deposited layers after spraying and of the powders used could be determined by means of X-ray diffraction (XRD).
  • advantageous effects of various embodiments of the invention can include, e.g., an increased service life of a zirconium-containing heat-insulating layer, achieved by the following steps: spraying heat-insulating-layer particles by means of APS with the selection of a sufficiently high current in combination with a plasma gas; simultaneously separately spraying MoSi 2 containing aluminum where the injection distance (I) is selected in combination with the spraying distance to ensure that the heat-insulating-layer material melts sufficiently in the plasma jet, and that the MoSi 2 powder supplied does melt, but without the material breaking down; and reducing an undesired volume expansion by using MoSi 2 powder in a maximum mass fraction of 5 wt. % based on the heat-insulating layer, preferably in a mass fraction of between 0.5 and 5 wt. %.
  • a number of tests indicating the success of systems and methods according to embodiments of the invention are set forth herein.
  • a MultiCoat APS system was used.
  • the cycling samples were coated in advance by means of VPS using an adhesion-promoter layer.
  • An F4 plasma-gas gun was used (all equipment from Oerlikon Metco, Wohlen, Switzerland).
  • VA steel was used as the substrate. This was roughened prior to coating by means of sandblasting in order to ensure that the heat-insulating layer bonded to the substrate.
  • Both Inconel 738 and Hastelloy X were used as the substrate material for the cycling samples.
  • the Hastelloy X substrates were used as the standard substrate. Amdry 365 from HC Starck GmbH, Goslar, Germany was consistently used as the adhesion-promoter layer.
  • both comparative layers (only YSZ) and the heat-insulating layer according to an embodiment of the invention were produced.
  • the current was 420 A in this process.
  • the spraying distance was set to 120 mm.
  • the injection distance (I) was 40 mm.
  • the MoSi 2 powder having an average particle diameter (d 50 ) of 33 ⁇ m was injected into the plasma jet by means of a conveying gas at 7 slpm.
  • a mixture of 46:4 slpm (Ar:He) was used as the plasma gas.
  • YSZ was used as the heat-insulating layer.
  • Amdry 365 was used as the adhesion-promoter layer.
  • the MoSi 2 mass fraction was 3 wt. % based on the YSZ heat-insulating layer.
  • the Al content in the MoSi 2 powder was 12 wt. %.
  • the service life of the MoSi 2 -YSZ mixed layer produced according to the invention was, at approx. 550 cycles (furnace cycling), approx. 260% higher than for a comparable, pure YSZ heat-insulating layer.
  • the recitation of “at least one of A, B and C” should be interpreted as one or more of a group of elements consisting of A, B and C, and should not be interpreted as requiring at least one of each of the listed elements A, B and C, regardless of whether A, B and C are related as categories or otherwise.
  • the recitation of “A, B and/or C” or “at least one of A, B or C” should be interpreted as including any singular entity from the listed elements, e.g., A, any subset from the listed elements, e.g., A and B, or the entire list of elements A, B and C.

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DE102016007231.8A DE102016007231A1 (de) 2016-06-15 2016-06-15 Selbst heilende Wärmedämmschichten sowie Verfahren zur Herstellung derselben
PCT/DE2017/000140 WO2017215687A1 (de) 2016-06-15 2017-05-23 Selbst heilende wärmedämmschichten sowie verfahren zur herstellung derselben

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CN113996783A (zh) * 2021-10-09 2022-02-01 中国航发北京航空材料研究院 裂纹愈合热障涂层粉体材料的制备方法
US11692274B2 (en) 2019-12-05 2023-07-04 Raytheon Technologies Corporation Environmental barrier coating with oxygen-scavenging particles having barrier shell

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NL2018995B1 (en) 2017-05-30 2018-12-07 Univ Delft Tech Self-healing particles for high temperature ceramics
CN111074190B (zh) * 2019-12-25 2021-12-21 江苏理工学院 一种钢材表面MoSi2复合涂层及其制备方法
CN113755784B (zh) * 2021-09-07 2024-03-26 浙江工业大学 一种基于超声振动辅助激光改性自愈合热障涂层的制备方法

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JPS56156754A (en) * 1980-05-06 1981-12-03 Mitsubishi Heavy Ind Ltd Composite material
JPS58153560A (ja) * 1982-03-10 1983-09-12 Komatsu Ltd 溶射皮膜形成方法
US6106903A (en) * 1999-03-01 2000-08-22 Plasma Technology, Inc. Thermal spray forming of molybdenum disilicide-silicon carbide composite material
EP1291449B1 (de) * 2001-08-03 2014-12-03 Alstom Technology Ltd Beschichtungsverfahren und beschichtetes reibungsbehaftetes Grundmaterial
CN101768380B (zh) * 2009-12-30 2014-12-17 中国科学院上海硅酸盐研究所 成分梯度变化的热防护涂层及制备方法
JP6125827B2 (ja) * 2012-12-20 2017-05-10 トーカロ株式会社 放射線遮蔽コーティング部材及び放射線遮蔽コーティング部材の製造方法
CN103553597B (zh) * 2013-10-30 2014-08-27 西安博科新材料科技有限责任公司 一种自愈合ysz陶瓷热障涂层材料及其制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11692274B2 (en) 2019-12-05 2023-07-04 Raytheon Technologies Corporation Environmental barrier coating with oxygen-scavenging particles having barrier shell
CN113996783A (zh) * 2021-10-09 2022-02-01 中国航发北京航空材料研究院 裂纹愈合热障涂层粉体材料的制备方法

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EP3472366A1 (de) 2019-04-24
CN109415795A (zh) 2019-03-01
WO2017215687A1 (de) 2017-12-21
JP2019519676A (ja) 2019-07-11
DE102016007231A1 (de) 2017-12-21
EP3472366B1 (de) 2020-10-14

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