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WO2000031313A1 - Materiau et procede pour produire une couche anticorrosion et anti-usure par metallisation a chaud - Google Patents

Materiau et procede pour produire une couche anticorrosion et anti-usure par metallisation a chaud Download PDF

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Publication number
WO2000031313A1
WO2000031313A1 PCT/EP1999/009140 EP9909140W WO0031313A1 WO 2000031313 A1 WO2000031313 A1 WO 2000031313A1 EP 9909140 W EP9909140 W EP 9909140W WO 0031313 A1 WO0031313 A1 WO 0031313A1
Authority
WO
WIPO (PCT)
Prior art keywords
control
online
magnetite
spray
material according
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.)
Ceased
Application number
PCT/EP1999/009140
Other languages
German (de)
English (en)
Inventor
Erich Lugscheider
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.)
JOMA CHEMICAL AS
Original Assignee
JOMA CHEMICAL AS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE19857737A external-priority patent/DE19857737A1/de
Application filed by JOMA CHEMICAL AS filed Critical JOMA CHEMICAL AS
Priority to EP99959337A priority Critical patent/EP1133580B1/fr
Priority to AU16550/00A priority patent/AU1655000A/en
Priority to AT99959337T priority patent/ATE239105T1/de
Priority to DE59905361T priority patent/DE59905361D1/de
Priority to JP2000584120A priority patent/JP2003522289A/ja
Publication of WO2000031313A1 publication Critical patent/WO2000031313A1/fr
Priority to NO20012564A priority patent/NO20012564D0/no
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • C23C4/06—Metallic material
    • 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
    • C23C4/11—Oxides
    • 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

Definitions

  • the invention relates to a material and a method for producing a corrosion and wear-resistant layer on a substrate by thermal spraying.
  • Corrosion and wear protection layers are usually applied from powder mixtures of various types to surfaces to be protected in manufacturing or for maintenance.
  • thermal spray processes or vapor deposition processes such as CVD (chemical vapor deposition) or PVD (plasma vapor deposition) are mainly used.
  • CVD chemical vapor deposition
  • PVD plasma vapor deposition
  • thin corrosion and wear protection layers based on oxide or hard material can be applied, especially in mass production.
  • Electrochemical or galvanic processes are also used.
  • Thermal spraying mainly creates layers with a layer thickness of more than 0.1 mm.
  • the corrosion and wear-resistant layers produced by thermal spraying are mostly metallic or oxidic layers in which hard materials are stored for improvement.
  • thermal spraying processes on substrates or parts with high quality requirements could only be used to a limited extent in series production.
  • the inventor has set himself the goal of improving the production of a constant wear-resistant and corrosion-resistant surface coating on an oxide basis by means of thermal spraying.
  • the layer material for producing the corrosion and wear-resistant layer has at least 20% by weight - preferably more than 30% by weight - magnetite iron (Fe 3 0 4 , also with additions of Fe 0 3 ); it can be pure magnetite (Fe 3 0 4 ) or a material made of magnetite and at least one further metallic material, possibly also magnetite and at least one intermetallic compound.
  • a material with an addition of carbide / s or nitride / s or silicide / s or boride / s or oxide / s has proven to be favorable or a material whose additions are mixtures of metals, intermetallic compounds, carbides, nitrides, suicides, Are borides and / or oxides.
  • the additions of up to 50% by weight, preferably up to 40% by weight, to the magnetic iron stone can be about Cr, CrNi or ferritic steels.
  • Carbides, nitrides, suicides, borides and oxides have proven their worth as additives for hard materials.
  • the carbide formers such as tungsten, chromium molybdenum, niobium, tantalum, titanium, vanadium or the like are suitable.
  • the addition of the carbides should be limited to a maximum of 30% by weight, preferably 20% by weight. With borides and nitrides as additives at this level, improvements in properties are observed.
  • Oxidic additions of chromium oxide (Cr 2 0 3 ) in the order of 1 to 40% by weight - preferably 5 to 30% by weight - also show good results.
  • the powdery spray materials In order to achieve high quality, the powdery spray materials must have a grain size of 0.05 to 150 ⁇ m - preferably 0.1 to 120 ⁇ m. When mixing different powdery materials, it is advisable to agglomerate or spray-dry to avoid segregation and to improve the flow behavior.
  • a cored wire When using wire-shaped spray materials with a high magnetite content, a cored wire can be produced from a metallic sheath and magnetite powder.
  • thermal spray processes such as autogenous flame spraying, high-speed flame spraying (HVOF spraying), plasma spraying under air (APS), Shroud plasma spraying (SPS), vacuum spraying (LPPS ), high-performance plasma spraying (HPPS), autogenous wire spraying or arc wire spraying can be used.
  • HVOF spraying high-speed flame spraying
  • APS plasma spraying under air
  • SPS Shroud plasma spraying
  • LPPS vacuum spraying
  • HPPS high-performance plasma spraying
  • autogenous wire spraying or arc wire spraying can be used.
  • the online control and control is carried out using a combination of different processes which allow the temperature of the particle or the degree of melting, the particle size, the speed, the impact of the same on the substrate and the heating of the layer and the substrate during the spraying process to eat.
  • the measurement signals are then fed to the computer of a control system for the spraying system and the flame parameters and the power are adapted to the values.
  • the inventor has thus found that it is possible to create a coating which meets the above-mentioned requirements if an iron-based oxide is used as the material, which - depending on the corrosion or wear problem to be solved - is used for metals, hard materials or intermetallic compounds.
  • the material must be produced using a specific manufacturing process; According to the invention, a powder grain with good flow properties, which is produced from the powdery material mixture by spray drying, is proposed, as well as a detachable powder grain made from the powdery material mixture by means of an agglomeration process.
  • the spraying system is equipped with an online control system for monitoring in order to be able to produce layers with a high quality and consistent properties by spraying.
  • the online control and control is conveniently used to measure the particle speed in the spray flame, for example by means of a laser Doppler anemometer using a beam emitted by a laser device, which is broken down into two partial beams by an optical transmitter.
  • the online temperature control monitors the particle temperature in the spray flame using a high-speed pyrometer. This is done using infrared thermography, for example.
  • Fig. 1 an online control and monitoring system for a plasma system
  • ITG infrared thermography
  • HSP High Speed Pyrometry
  • Fig. 3 a scheme for infrared thermography (ITG);
  • HSP Pyrometry
  • LDA laser Doppler anemometer
  • Fig. 7 a sketch for particle shape measurement in flight
  • PTM Particle Temperature Measurement
  • Fig. 9 a sketch for measuring the particle temperature and speed.
  • thermal spray processes are used to apply wear and / or corrosion layers - such as autogenous flame spraying, high-speed flame spraying (HVOF), plasma spraying under air (APS), so-called Shroud plasma spraying (SPS), plasma spraying in a vacuum (LPPS), high-power plasma spraying (HPPS), autogenous or arc wire spraying - applicable.
  • the online control and control takes place by means of a combination of different processes, which allow the temperature of the particle or the degree of melting, the particle size, the speed, the impact of the same on the substrate as well as the heating of the layer and the substrate during the spraying process to eat.
  • the measurement signals are then fed to the computer of the control part of the thermal spray system in order to be able to adapt the flame parameters and the power to the measured values.
  • FIG. 1 An online control and monitoring system shown in FIG. 1 for the flame or the spray jet 10 of a spray gun or the like indicated at 12.
  • LDA - detector
  • FIG. 3 To measure substrate temperature T s and coating temperature T c by means of infrared thermography, according to FIG. 3 there is a substrate 30 - to be provided with a coating 32 - in the recording area of an ITG camera 18.
  • a glass fiber cable 36 extends from the latter one indicated at 42 indicated video PC card - 500 kHz.
  • a computer 46 with a monitor 48 is connected to this, to which a temperature recording device 50 is assigned here.
  • the coating 32 of the substrate 30 is connected to the HSP head 24, which has an AD converter 52 to a storage element 44 and monitor 48 - Computer 46 is connected.
  • the process of laser Doppler anemometry (LDA) can be used to optimize the spray parameters with little time and effort.
  • the modulation frequency of the scattered light signal 68 is proportional to the speed component of the particle perpendicular to the interference fringe system.
  • the frequency of the LDA scattered light signals is a measure of the local density of the particles in the plasma spray jet 10. A locally resolved measurement of relevant particle parameters is possible by scanning the beam. Results such as speed distribution, trajectories and dwell times of the particles can be obtained from this.
  • PSD particle-shape imaging
  • the image recording system consists of a CCD camera 78 with an upstream micro-channel plate (MCP) image intensifier with a minimum exposure time of 5 ns.
  • MCP micro-channel plate
  • in-flight particle diagnosis method to which reference is made to FIG. 8 - up to 200 individual particles per second can be measured simultaneously at each point of a spray jet for their surface temperature, speed and size, regardless of the spraying method .
  • a non-reproduced travel unit additionally enables a plane to be scanned perpendicular to the spray jet 10, so that the distribution of the particles in the spray jet 10 can be determined precisely.
  • the temperature is determined using two-wavelength pyrometery at 995 ⁇ 25 ⁇ m and 787 ⁇ 25 ⁇ m.
  • the particles are treated as gray emitters so that knowledge of the exact emissivity is not necessary for the temperature measurement.
  • the system comprises imaging a two-slit mask 80 with 25 ⁇ m ⁇ 50 ⁇ m — on a measuring head 82 — at a focal point at a distance of approximately 90 mm with a high depth of field.
  • This creates a measurement volume which, according to the graphic representation in FIG. 10, is characterized by two visible and one shadow region in between.
  • the measuring volume is approximately 170 x 250 x 2000 ⁇ m 3 .
  • the natural radiation of individual particles that fly through this measurement volume is detected by two IR detectors recorded with two different wavelengths.
  • the two partial measurement volumes result in two temperature peaks in a row.
  • the time interval between the two peaks is a measure of the speed of the particle.
  • the principle corresponds to that of the light barrier.
  • the measurable particle size essentially depends on the temperature of the particles. It has a lower limit of approximately 10 ⁇ m and an upper limit of approximately 300 ⁇ m and is determined by the absolute energy radiated by the particle, which is proportional to the square of the diameter.
  • the measurable speed range is 30m / s - 1500 m / s.
  • FIG. 9 follows on from that in FIG. 1 and illustrates the measurement of the particle temperature and the speed by means of an HSP head 24.
  • a casting mold for aluminum casting should be provided with a layer that prevents caking and sticking in the mold.
  • the grain structure of the round grains was produced by agglomeration by means of spray drying.
  • the application was carried out by plasma spraying under air (APS) with a power of 60 KW and argon / hydrogen plasma, which was provided with an online control unit according to FIG. 1;
  • the particle speed and particle temperature are measured there during the flight in order to control the plasma spray jet in such a way that the necessary degree of melting of the particle is achieved.
  • the mold surface to be coated was forced-cooled with CO 2 with the aim of keeping the oxidation upon particle impact as low as possible.
  • the layer thus produced by thermal spraying was then ground and tested in an aluminum foundry. It was found that caking and sticking to the mold is prevented and the time-consuming spraying of the mold with a mold release agent can be avoided.
  • the grain size of the starting material for the filling was> 1.0 ⁇ m.
  • an arc spraying system equipped with an online control and control system was used for processing cored wire, and a control system was a combination of the two systems shown in FIGS. 1 and 3.
  • the forced cooling is done with C0 and air.
  • the 200 cm long roll was ground to a surface quality of Ra 0.4 ⁇ m.
  • the grain size of the wettable powder was: ⁇ 37 ⁇ m> 5 ⁇ m
  • the spray powder with a round grain shape was produced by agglomeration during spray drying.
  • C0 2 was used as forced cooling for the substrate and the layer during the spraying process.
  • the Shroud used to protect against oxidation was operated with pure starch.
  • the piston rings coated with pure magnetite using this method showed high quality when checked and showed good results in the endurance test in engines.
  • a dipping device for a salt bath working at 500 ° C. for the heat treatment of smaller parts shows high corrosion after approximately one week of operation.
  • the thermal spraying process for applying the layer with a thickness of 80 ⁇ m was a high-speed flame spraying (HVOF), in which the control was carried out online. After spraying, the layer was polished.
  • HVOF high-speed flame spraying
  • a hydraulic cylinder for underground mining with a length of 1000 mm and a diameter of 200 mm should be provided with a protective layer against corrosion and wear.
  • a galvanically applied hard chrome layer had been used as a protective layer, but due to the occurrence of hairline cracks in the layer, it had a service life of at most two months.
  • an HPPS (High Power Plasma) system with an output of 200 KW was used, which was used to maintain the exact spray parameters and avoid oxidation with an online control was provided.
  • the protective layer thus prepared was checked after a period of two months, and it was found that the surface of the layer showed no attacks by corrosion or wear. The lifespan of the layer was nine months.
  • the piston of a vacuum pump with a diameter of 20 mm and a length of 500 mm should be provided with a wear and corrosion protection layer.
  • An LPPS system with an output of 40 KW was used for coating, which was provided with an online control.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)

Abstract

L'invention concerne un matériau utilisé pour produire une couche anticorrosion et anti-usure sur un substrat, par métallisation à chaud. Ce matériau comprend au moins 20 % en poids, de préférence plus de 30 % en poids de pierre d'aimant (Fe3O4 et/ou FeFe2O4). Ce matériau consiste de préférence en magnétite pure ou en magnétite et en au moins un autre matériau métallique ou en au moins un composé intermétallique.
PCT/EP1999/009140 1998-11-25 1999-11-25 Materiau et procede pour produire une couche anticorrosion et anti-usure par metallisation a chaud Ceased WO2000031313A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
EP99959337A EP1133580B1 (fr) 1998-11-25 1999-11-25 Procede pour produire une couche anticorrosion et anti-usure par metallisation a chaud
AU16550/00A AU1655000A (en) 1998-11-25 1999-11-25 Material for producing a corrosion- and wear-resistant layer by thermal spraying
AT99959337T ATE239105T1 (de) 1998-11-25 1999-11-25 Verfahren zum herstellen einer korrosions- und verschleissfesten schicht durch thermisches spritzen
DE59905361T DE59905361D1 (de) 1998-11-25 1999-11-25 Verfahren zum herstellen einer korrosions- und verschleissfesten schicht durch thermisches spritzen
JP2000584120A JP2003522289A (ja) 1998-11-25 1999-11-25 溶射により耐食および耐摩耗層を形成する材料および方法
NO20012564A NO20012564D0 (no) 1998-11-25 2001-05-25 Materiale og fremgangsmåte for fremstilling av et korrosjons- og slitasjebestandig lag ved termisk spröyting

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE19854512 1998-11-25
DE19854512.6 1998-11-25
DE19857737.0 1998-12-15
DE19857737A DE19857737A1 (de) 1998-11-25 1998-12-15 Werkstoff und Verfahren zum Herstellen einer korrosions- und verschleißfesten Schicht durch thermisches Spritzen

Publications (1)

Publication Number Publication Date
WO2000031313A1 true WO2000031313A1 (fr) 2000-06-02

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PCT/EP1999/009140 Ceased WO2000031313A1 (fr) 1998-11-25 1999-11-25 Materiau et procede pour produire une couche anticorrosion et anti-usure par metallisation a chaud

Country Status (6)

Country Link
EP (1) EP1133580B1 (fr)
JP (1) JP2003522289A (fr)
AT (1) ATE239105T1 (fr)
AU (1) AU1655000A (fr)
NO (1) NO20012564D0 (fr)
WO (1) WO2000031313A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1290238A1 (fr) * 2000-05-23 2003-03-12 Joma Chemical AS Materiau et procede pour realiser une couche resistante a la corrosion et a l'usure par projection thermique
WO2004029319A3 (fr) * 2002-09-21 2004-05-27 Mtu Aero Engines Gmbh Procede pour revetir une piece
US6952971B2 (en) 2000-08-23 2005-10-11 Schenck Process Gmbh Apparatus for measuring a mass flow
US6964846B1 (en) 1999-04-09 2005-11-15 Exact Sciences Corporation Methods for detecting nucleic acids indicative of cancer
US11745201B2 (en) 2012-06-11 2023-09-05 General Electric Company Spray plume position feedback for robotic motion to optimize coating quality, efficiency, and repeatability

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE59909522D1 (de) * 1999-01-19 2004-06-24 Sulzer Metco Ag Wohlen Durch Plasmaspritzen aufgebrachte Schicht für Zylinderlaufflächen von Motorblöcken und Verfahren zu deren Herstellung
CH694664A5 (de) * 2000-06-14 2005-05-31 Sulzer Metco Ag Durch Plasmaspritzen eines Spritzpulvers aufgebrachte eisenhaltige Schicht auf einer Zylinderlauffläche.
KR20230102606A (ko) * 2021-12-30 2023-07-07 이창훈 플라즈마 서스펜션 코팅 시스템 및 방법

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US2707691A (en) * 1952-08-08 1955-05-03 Norton Co Coating metals and other materials with oxide and articles made thereby
DE2258405A1 (de) * 1971-12-04 1973-06-07 Nippon Piston Ring Co Ltd Verfahren zur herstellung einer gegen abnutzung bzw. abrieb widerstandsfaehigen, der gleitreibung ausgesetzten oberflaeche
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JPH08225911A (ja) * 1995-02-15 1996-09-03 Tocalo Co Ltd 耐久性に優れる溶射被覆電極およびその製造方法
JPH08269672A (ja) * 1995-03-30 1996-10-15 Toshiba Corp 溶射皮膜の評価方法および装置
DE19545005A1 (de) * 1995-12-02 1997-06-05 Abb Patent Gmbh Verfahren zur Überwachung der Beschichtung einer Platte aus einem Metall mit hoher Leitfähigkeit mit einem Material mit geringerer Leitfähigkeit und Vorrichtung zur Durchführung des Verfahrens
EP0837305A1 (fr) * 1996-10-21 1998-04-22 Sulzer Metco AG Méthode et assemblage pour contrÔler le processus de revêtement dans un dispositif de revêtement thermique
EP0955389A1 (fr) * 1998-05-06 1999-11-10 Linde Aktiengesellschaft ContrÔle de qualité pour un procédé de pulvérisation thermique

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6964846B1 (en) 1999-04-09 2005-11-15 Exact Sciences Corporation Methods for detecting nucleic acids indicative of cancer
EP1290238A1 (fr) * 2000-05-23 2003-03-12 Joma Chemical AS Materiau et procede pour realiser une couche resistante a la corrosion et a l'usure par projection thermique
US6952971B2 (en) 2000-08-23 2005-10-11 Schenck Process Gmbh Apparatus for measuring a mass flow
WO2004029319A3 (fr) * 2002-09-21 2004-05-27 Mtu Aero Engines Gmbh Procede pour revetir une piece
US11745201B2 (en) 2012-06-11 2023-09-05 General Electric Company Spray plume position feedback for robotic motion to optimize coating quality, efficiency, and repeatability

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EP1133580A1 (fr) 2001-09-19
AU1655000A (en) 2000-06-13
ATE239105T1 (de) 2003-05-15
JP2003522289A (ja) 2003-07-22
NO20012564L (no) 2001-05-25
NO20012564D0 (no) 2001-05-25
EP1133580B1 (fr) 2003-05-02

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