EP1899494B1 - Procede de fabrication de couches ceramiques - Google Patents

Procede de fabrication de couches ceramiques Download PDF

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Publication number
EP1899494B1
EP1899494B1 EP06763866A EP06763866A EP1899494B1 EP 1899494 B1 EP1899494 B1 EP 1899494B1 EP 06763866 A EP06763866 A EP 06763866A EP 06763866 A EP06763866 A EP 06763866A EP 1899494 B1 EP1899494 B1 EP 1899494B1
Authority
EP
European Patent Office
Prior art keywords
particles
precursors
ceramic
process according
gas jet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Not-in-force
Application number
EP06763866A
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German (de)
English (en)
Other versions
EP1899494A2 (fr
Inventor
Ursus KRÜGER
Raymond Ullrich
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Siemens AG
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Siemens AG
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Filing date
Publication date
Application filed by Siemens AG filed Critical Siemens AG
Publication of EP1899494A2 publication Critical patent/EP1899494A2/fr
Application granted granted Critical
Publication of EP1899494B1 publication Critical patent/EP1899494B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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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
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/02—Coating starting from inorganic powder by application of pressure only
    • C23C24/04—Impact or kinetic deposition of particles

Definitions

  • the invention relates to a method for producing ceramic layers, in which particles are injected by means of a nozzle onto the surface to be coated and adhere there.
  • thermal spraying The production of ceramic layers by thermal spraying is known, for example, from a publication of the US Department of Defense ( The AMPTIAC Newsletter, Spring 2002, Vol. 1 ). Thereafter, microparticles containing the ceramic constituents of the ceramic coating to be produced can be sprayed onto the surface to be coated in a thermal spraying process.
  • a plasma jet is generated, in which the microparticles of the ceramic material are fed and thereby at least partially melted.
  • a ceramic structure is formed, which may possibly be completed by a thermal aftertreatment.
  • siliceous plastics also referred to as preceramic polymers (eg, polycarbosilanes, polysilazanes, and polysiloxanes)
  • preceramic polymers eg, polycarbosilanes, polysilazanes, and polysiloxanes
  • thermal decomposition pyrolysis
  • thermo spraying HVOF spraying
  • the thermally sensitive polymer material is processed as particles which are encased by the ceramic material to be embedded. These particles may be in the flame jet of the thermal Spraying method are introduced so that the desired polymer-ceramic composite is formed in the sprayed layer.
  • the object of the invention is to provide a method for producing ceramic layers by means of injection, which is accessible to the production of polymer-ceramic layers.
  • This object is achieved with the method mentioned in the present invention that are used as particles precursors of a polymer ceramic (which are also referred to as preceramic polymers) and used as a nozzle Kaltspritzdüse using cold spraying.
  • the use of the cold spraying method has the advantage that, in contrast to thermal spraying processes, the energy required to form the coating is produced due to a strong acceleration of the coating particles in the cold gas jet (preferably at a multiple speed of sound).
  • Cold spraying are basically for example from the DE 102 24 780 A1 known.
  • the device necessary for operating the method has, for example, a vacuum chamber in which a substrate can be placed in front of a so-called cold spray nozzle.
  • the vacuum chamber is evacuated and by means of the cold spray nozzle (also called cold gas spray gun) a gas jet is generated, in which particles can be introduced for coating the workpiece.
  • the cold spray nozzle also called cold gas spray gun
  • the particles can additionally be heated, their heating being limited in such a way that the melting temperature of the particles is not achieved (this circumstance is named after the term cold gas spraying).
  • the energy input into the coating particles can be changed by adjusting the speed of the cold gas jet and by possibly additional introduction of thermal energy in the cold gas jet. It must be dimensioned so that the precursors of the polymer ceramic, which are accelerated in particle form on the surface of the substrate to be coated, at least adhere (see below for more). As a result, a coating of polymer ceramic can be produced by spraying, the properties of which are not jeopardized by thermal overstressing of the particles to be sprayed.
  • fillers whose thermal sensitivity would not permit an addition to the plasma jet of a thermal spraying process. Since the ceramics used in thermal spraying generally have a very high melting point, the addition of fillers is virtually eliminated in conventional ceramic processes.
  • metals in particular zirconium (Zr), titanium (Ti) or aluminum (A1) or metal alloys are supplied, in particular, from the abovementioned materials, which react with the precursors of the polymer ceramic during layer formation. This creates the opportunity to influence the composition of the polymer ceramics by adding active fillers.
  • passive fillers for example silicon oxide (SiO 2 ), silicon carbide (SiC), silicon nitride (SiN), boron nitride (BN) or corundum.
  • passivated or inactive metal alloys or metals can be added. Passivated metals are inactive because they have an oxidized surface that has ceramic properties. Inactive metals generally have a sufficiently high melting point that they are not involved in the reactions involved in the formation of the polymer ceramic. Priority is given to noble metals such as gold (Au) or platinum (Pt).
  • the fillers may preferably be incorporated nanoparticulate in the cold spraying process.
  • the nanoparticles In order to enable processing with cold gas spraying, the nanoparticles must be bound to larger particles due to their very low inertia.
  • the fillers can be embedded as nanoparticles in a matrix preceramic polymer as precursors of the polymer ceramic, wherein the precursors each form microparticles that can be processed with the cold gas spraying. Embedding in the matrix of the precursors is particularly advantageous in the case of reactive fillers, since they can then react completely in the formation process of the polymer ceramic because of their good distribution and large surface area.
  • a process for producing microparticles with nanoparticles embedded in a matrix as a microencapsulation is offered, for example, by the company Capsulation®.
  • the energy input into the cold gas jet is dimensioned in this way is that the reaction of the precursors of Polymerkerämik is completed during the film formation.
  • the precursors of the polymer ceramic are completely converted into the polymer ceramic when hitting the substrate (substrate or layer under construction), and fillers are incorporated at the same time or react with the precursors of the polymer ceramic.
  • the energy input into the cold gas jet is dimensioned such that adhesion of the particles is ensured, however, the reaction of the precursors of the polymer ceramic is not completed and then a post-treatment takes place.
  • the post-treatment can advantageously be carried out targeted conversion into polymer ceramics, which is done in the entire layer composite generated, whereby the construction of manufacturing-related stresses can be advantageously reduced or even excluded.
  • Aftertreatment in this context should also be understood to mean a treatment initiated directly after the impingement of the precursors of the polymer ceramic, which already applies additional energy to the formed portion of the coating during the layer construction.
  • the aftertreatment is effected, for example, by the energy input of electromagnetic radiation, in particular of laser light, into the layer which forms.
  • the laser can be advantageously aligned with the impact of the cold gas jet, which is achieved by the energy input into the layer just as locally, as is achieved by the cold gas jet.
  • the polymer ceramic in the coating can also be completed when, due to the requirements of the process, the energy input into the cold gas jet is limited.
  • the process parameter of the energy input into the cold gas jet can also advantageously be used to favorably influence the adhesion of the layer to the substrate. This happens because the energy input into the cold gas jet during the coating of the still uncoated substrate is dimensioned such that the particles form a bond with the material of the substrate. In this case, the fact must be taken into account that due to their kinetic energy, the particles can form a bond with the substrate when they are still uncoated, and these can consist, for example, of covalent bonds. As a result, the layer adhesion is advantageously improved, which, for example, reduces the risk of it peeling off when the ceramic layer is subjected to mechanical stress.
  • the single FIGURE represents a device for cold gas spraying.
  • This has a vacuum container 11, in which on the one hand a cold spray nozzle 12, which can also be referred to as a cold gas spray gun, and on the other hand, a substrate 13 is arranged (attachment not shown).
  • a process gas of the cold gas spray gun 12 can be supplied.
  • This has, as indicated by the contour, a Lavalform, through which the process gas is expanded and accelerated in the form of a gas jet (arrow 15) to a surface 16 of the substrate 13 out.
  • the process gas can, for example, as Reactive gas containing oxygen 17.
  • the process gas can be heated in a manner not shown, whereby a required process temperature is established in the vacuum container 12.
  • particles 19 can be supplied, which can be designed as a matrix preceramic polymers 19a with fillers 19b for the polymer ceramic to be formed. These particles are accelerated in the gas jet and impinge on the surface 16. The kinetic energy of the particles causes them to adhere to the surface 16, whereby the oxygen 17 is also incorporated into the forming layer 20 or participates in the pyrolytic reactions of the preceramic polymers.
  • further filler particles 19 c which are designed as microparticles, the cold gas jet are mixed, which are also incorporated in the layer 21.
  • the substrate 13 can be moved back and forth in the direction of the double arrow 21 in front of the cold spray nozzle 12.
  • the vacuum in the vacuum chamber 11 is constantly maintained by the vacuum pump 22, wherein the process gas is passed through a filter 23 before being passed through the vacuum pump 22 to filter out particles which were not bonded to the surface 16 upon impact with the surface 16 ,
  • a boundary region 24 which is shown cross-hatched and refers to the part of the structure of the substrate 13 adjoining the surface 16 and the particles of the forming layer adjoining the surface.
  • a heater 25 is furthermore provided in the vacuum container 11. With this, during the course of the coating process, the temperatures required in the vacuum chamber can be achieved. Furthermore, to introduce a local energy input into the layer in the form of electromagnetic radiation, a laser is accommodated in the vacuum container 11, which can be moved by means of a pivotable suspension. In particular, this can, as shown in the figure, be aligned with the impact point of the cold gas jet 15, whereby an additional external energy input can take place during the layer formation process, which is independent of the energy input into the cold gas jet 15.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Claims (8)

  1. Procédé de production de couches ( 20 ) en céramique, dans lequel on pulvérise des particules ( 19 ) au moyen d'une buse sur la surface ( 16 ) à revêtir et on les y laisse adhérer,
    caractérisé
    en ce qu'on utilise comme particules des précurseurs ( 19a ) d'une céramique polymère constituée sous la forme de polymères pré-céramiques et on utilise, comme buse, une buse ( 12 ) de projection à froid en mettant en oeuvre la projection de gaz froid.
  2. Procédé suivant la revendication 1,
    caractérisé
    en ce que l'on apporte d'autres particules comme charge ( 19b, 19c ) au jet ( 15 ) de gaz froid produit par la buse.
  3. Procédé suivant la revendication 2,
    caractérisé
    en ce que l'on apporte des métaux ou des alliages de métaux comme charge ( 19b, 19c ) active, qui réagissent lors de la formation de la couche sur les précurseurs ( 19a ) de la céramique polymère.
  4. Procédé suivant la revendication 2 ou 3,
    caractérisé
    en ce que l'on apporte des céramiques ou des alliages métalliques ou des métaux inactifs ou passivés comme charge ( 19a, 19c ) passives qui, lors de la formation de la couche, restent sans participer à la réaction des précurseurs ( 19a ) de la céramique polymère.
  5. Procédé suivant l'une des revendications précédentes,
    caractérisé
    en ce qu'on proportionne l'apport d'énergie au jet ( 15 ) de gaz froid, de manière à exclure complètement la réaction des précurseurs ( 19a ) de la céramique polymère pendant la formation de la couche.
  6. Procédé suivant l'une des revendications 1 à 3,
    caractérisé
    en ce que l'on proportionne l'apport d'énergie au jet ( 15 ) de gaz froid, de manière à assurer une adhérence des particules ( 19 ), mais à ne pas exclure la réaction des précurseurs ( 19a ) de la céramique polymère et on effectue ensuite un post-traitement.
  7. Procédé suivant la revendication 6,
    caractérisé
    en ce que l'on effectue le post-traitement par l'apport d'énergie de rayonnement électromagnétique à la couche qui se forme.
  8. Procédé suivant l'une des revendications précédentes,
    caractérisé
    en ce que l'on proportionne l'apport d'énergie au jet ( 15 ) de gaz froid lors du revêtement du substrat ( 13 ) qui n'est pas encore revêtu, de manière à ce que les particules ( 19 ) entrent en liaison avec le matériau du substrat ( 13 ).
EP06763866A 2005-06-28 2006-06-23 Procede de fabrication de couches ceramiques Not-in-force EP1899494B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005031101A DE102005031101B3 (de) 2005-06-28 2005-06-28 Verfahren zum Herstellen von keramischen Schichten
PCT/EP2006/063516 WO2007000422A2 (fr) 2005-06-28 2006-06-23 Procede de fabrication de couches ceramiques

Publications (2)

Publication Number Publication Date
EP1899494A2 EP1899494A2 (fr) 2008-03-19
EP1899494B1 true EP1899494B1 (fr) 2010-07-28

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP06763866A Not-in-force EP1899494B1 (fr) 2005-06-28 2006-06-23 Procede de fabrication de couches ceramiques

Country Status (5)

Country Link
US (1) US7781024B2 (fr)
EP (1) EP1899494B1 (fr)
JP (1) JP5106390B2 (fr)
DE (2) DE102005031101B3 (fr)
WO (1) WO2007000422A2 (fr)

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US8192799B2 (en) * 2008-12-03 2012-06-05 Asb Industries, Inc. Spray nozzle assembly for gas dynamic cold spray and method of coating a substrate with a high temperature coating
US8020509B2 (en) * 2009-01-08 2011-09-20 General Electric Company Apparatus, systems, and methods involving cold spray coating
DE102009033620A1 (de) * 2009-07-17 2011-01-20 Mtu Aero Engines Gmbh Kaltgasspritzen von oxydhaltigen Schutzschichten
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DE102011052118A1 (de) * 2011-07-25 2013-01-31 Eckart Gmbh Verfahren zum Aufbringen einer Beschichtung auf einem Substrat, Beschichtung und Verwendung von Partikeln
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US10792679B2 (en) 2018-04-17 2020-10-06 General Electric Company Coating system and method
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CN109554701B (zh) * 2018-12-27 2021-06-29 东莞华誉精密技术有限公司 一种手机壳体表面的喷涂方法及喷涂装置
DE102019218273A1 (de) * 2019-11-26 2021-05-27 Siemens Aktiengesellschaft Kaltgas-Spritzanlage mit einer Heizgasdüse und Verfahren zum Beschichten eines Substrats
CN115400926B (zh) * 2021-05-27 2024-05-10 创兆光有限公司 半导体激光器介电层以及半导体激光器的制作方法
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Also Published As

Publication number Publication date
JP5106390B2 (ja) 2012-12-26
EP1899494A2 (fr) 2008-03-19
DE502006007540D1 (de) 2010-09-09
JP2008544092A (ja) 2008-12-04
WO2007000422A2 (fr) 2007-01-04
US7781024B2 (en) 2010-08-24
WO2007000422A3 (fr) 2007-03-22
US20090202732A1 (en) 2009-08-13
DE102005031101B3 (de) 2006-08-10

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