DE1109482B - Process for the production of siliconizing layers - Google Patents
Process for the production of siliconizing layersInfo
- Publication number
- DE1109482B DE1109482B DEM41076A DEM0041076A DE1109482B DE 1109482 B DE1109482 B DE 1109482B DE M41076 A DEM41076 A DE M41076A DE M0041076 A DEM0041076 A DE M0041076A DE 1109482 B DE1109482 B DE 1109482B
- Authority
- DE
- Germany
- Prior art keywords
- silicon
- copper
- layers
- molybdenum
- melt
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims description 11
- 238000005475 siliconizing Methods 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 17
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 239000010949 copper Substances 0.000 claims description 17
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 15
- 229910052750 molybdenum Inorganic materials 0.000 claims description 15
- 239000011733 molybdenum Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000011133 lead Substances 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 239000003870 refractory metal Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 239000011135 tin Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910000881 Cu alloy Inorganic materials 0.000 claims 1
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 claims 1
- 238000009792 diffusion process Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 16
- 239000000155 melt Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- -1 silicon silicates Chemical class 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/18—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions
- C23C10/20—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions only one element being diffused
- C23C10/22—Metal melt containing the element to be diffused
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Description
Verfahren zur Herstellung von Silizierungsschichten In den letzten Jahren haben Molybdän und Molybdänlegierungen infolge ihrer hohen Warmfestigkeit steigendes Interesse als Material für Turbinenschaufeln, Brennkammerauskleidungen, Raketendüsen sowie als Heizleitermaterial gefunden.Process for the production of siliconization layers In the last Years, molybdenum and molybdenum alloys have due to their high heat resistance increasing interest as a material for turbine blades, combustion chamber linings, Rocket nozzles and found as heat conductor material.
Diese Warmfestigkeit des Molybdäns bzw. seiner Legierungen (z. B. Mo-Ti, Mo-W, Mo-Ta usw.) kann aber an oxydierender Atmosphäre, z. B. an Luft, nur ausgenutzt werden, wenn das Molybdän durch das Aufbringen von zunderfesten Oberflächenschichten gegen die starke Korrosion durch Oxydation geschützt wird. Als besonders günstig in bezug auf Oxydationsschutzwirkung haben sich Überzüge aus Molybdänsilizid bewährt, die an Luft einen Oxydationsschutz bis 1700° C ergeben, was besonders für Molybdänheizleiter wichtig ist, die in elektrischen Öfen mit oxydierender Atmosphäre angeordnet sind.This high temperature strength of molybdenum or its alloys (e.g. Mo-Ti, Mo-W, Mo-Ta, etc.) can, however, in an oxidizing atmosphere, e.g. B. in air, only can be used when the molybdenum is deposited by the application of scale-resistant surface layers is protected against strong corrosion by oxidation. As particularly cheap With regard to the anti-oxidation effect, coatings made of molybdenum silicide have proven effective, which provide protection against oxidation up to 1700 ° C in air, which is especially good for molybdenum heating elements is important, which are placed in electric furnaces with an oxidizing atmosphere.
Das Auftragen von Silizidschichten als zunderfester Oberflächenschutz hat nicht nur Bedeutung bei Molybdän und seinen Legierungen, sondern auch bei den anderen warmfesten, aber nicht oxydationsbeständigen Metallen wie Wolfram, Tantal, Niob und deren Legierungen. Silizierungsschichten sind außerdem wichtig als korrosionsfeste Schichten, besonders gegen den Säureangriff bei Eisen, Stahl, Nickel und Nickellegierungen.The application of silicide layers as scale-resistant surface protection is important not only for molybdenum and its alloys, but also for the other heat-resistant, but not oxidation-resistant metals such as tungsten, tantalum, Niobium and their alloys. Silicating layers are also important as corrosion-resistant Layers, especially against acid attack on iron, steel, nickel and nickel alloys.
Die Silizierungsschichten wurden bisher auf die metallischen Formteile so aufgetragen, daß die zu silizierenden Teile in Siliziumschmelzen eingetaucht wurden. Nach anderen Verfahren wird Silizium aufgesprizt, aufgedampft oder in Pulverform aufgetragen und durch nachherige thermische Behandlung mit dem Grundmaterial zur Reaktion gebracht. Es ist auch möglich, die zu behandelnden Teile in Siliziumpulver eingebettet zu glühen, und schließlich können die Formteile durch Glühen in einer Schutzgasatmosphäre, die gasförmige Siliziumverbindungen enthält, siliziert werden.The siliconizing layers have so far been applied to the metallic moldings applied in such a way that the parts to be siliconized are immersed in silicon melts became. According to other methods, silicon is sprayed on, vapor-deposited or in powder form applied and by subsequent thermal treatment with the base material for Brought reaction. It is also possible to put the parts to be treated in silicon powder embedded to anneal, and finally the molded parts by annealing in a Protective gas atmosphere, which contains gaseous silicon compounds, are siliconized.
Schließlich ist auch ein Verfahren zur Herstellung eines oxydationsbeständigen Überzuges auf einem aus mindestens 50 % Molybdän bestehenden Gegenstand bereits bekanntgeworden, gemäß welchem auf den Gegenstand ein Aluminium und Silizium enthaltender Überzug aufgebracht und der überzogene Gegenstand unter Molybdän nicht oxydierenden Bedingungen auf einer erhöhten Temperatur gehalten wird, um zwischen dem Überzug und dem darunterliegenden Metall eine Diffusion zu bewirken, wodurch ein nicht oxydierter Überzug aus Aluminium, Silizium und Molybdän gebildet wird.Finally, there is also a method of making one that is resistant to oxidation Coating on an object consisting of at least 50% molybdenum already became known, according to which on the object an aluminum and silicon containing Coating applied and the coated object under molybdenum non-oxidizing Conditions at an elevated temperature is maintained between the coating and causing the underlying metal to diffuse, thereby creating a non-oxidized Coating is formed from aluminum, silicon and molybdenum.
Die Erfindung zeigt nun einen Weg zur Herstellung von Silizierungsschichten, durch den alle bisher auftretenden Mängel solcher Schichten, wie ungünstig hohe Silizierungstemperatur, die im Falle des Molybdäns zu einer ungünstigen Herabsetzung der mechanischen Eigenschaften führt, sowie Ungleichmäßigkeiten der Silizierungsschicht vermieden werden. Das erfindungsgemäße Verfahren besteht darin, daß der zu silizierende Formkörper aus hochschmelzenden Metallen, insbesondere aus Molybdän, Wolfram, Tantal, Niob und deren Legierungen der Einwirkung einer siliziumhaltigen Kupferschmelze ausgesetzt werden. Kupfer vermag Silizium aufzulösen, reagiert aber mit dem zu silizierenden Metall wenig oder überhaupt nicht.The invention now shows a way of producing siliconizing layers, due to all the deficiencies of such layers that have occurred so far, such as unfavorably high Siliconization temperature, which in the case of molybdenum leads to an unfavorable reduction mechanical properties, as well as irregularities in the siliconization layer be avoided. The inventive method consists in that the siliconized Shaped bodies made of refractory metals, in particular made of molybdenum, tungsten, tantalum, Niobium and its alloys from the action of a silicon-containing copper melt get abandoned. Copper can dissolve silicon, but reacts with the silicon to be siliconized Little or no metal.
Bei Ausübung des Verfahrens hat es sich von besonderem Vorteil gezeigt, die zu silizierenden Formteile in die siliziumhaltige Kupferschmelze einzutauchen. Man kann aber auch die siliziumhaltige Kupferschmelze auf die Formkörper durch Aufspritzen, Aufdampfen oder Aufbringen in Pulverform auftragen, worauf zur Ausbildung der Silizierungsschicht eine thermische Nachbehandlung erfolgt.When performing the procedure, it has been shown to be particularly advantageous to immerse the molded parts to be siliconized in the silicon-containing copper melt. However, the silicon-containing copper melt can also be sprayed onto the molded body, Apply vapor deposition or application in powder form, followed by the formation of the siliconized layer thermal post-treatment takes place.
Bei der Einwirkung der Schmelze siliziert das gelöste Silizium das zu silizierende Metall. Durch eine chemische oder elektrochemische Beizung wird dann nach dem Herausnehmen des silizierten Metallformteiles aus der Schmelze und nach dem Abkühlen die noch anhaftende siliziumhaltige Kupferschmelze entfernt, während die Silizierungsschicht festhaftend und gleichmäßig auf der Oberfläche des Metallformteiles verbleibt.When the melt acts, the dissolved silicon silicates the metal to be siliconized. With a chemical or electrochemical pickling then after removing the siliconized metal molding the melt and, after cooling, the silicon-containing copper melt that is still adhering removed while the siliconizing layer adheres firmly and evenly to the surface of the molded metal part remains.
Werden z. B. Mo-Stäbe in die siliziumhaltige Kupferschmelze eingetaucht, so wird das Molybdän an der Oberfläche durch- das- gelöste Silizium in Molybdänsilizid umgewandelt, während das Kupfer nicht mit dem Molybdän reagiert. Die aus der Schmelze herausgenommenen Molybdänstäbe werden dann mit verdünnter Salpetersäure behandelt, wodurch das mechanisch festhaftende Kupfer gleichzeitig mit dem im Kupfer gelösten, nicht für den Aufbau der Molybdänsilizidschicht verbrauchten Siliziam vollständig entfernt wird. Die Molybdänsilizidschicht wird dabei nicht angegriffen und verbleibt als gleichmäßig dicke, festhaftende Schicht auf der Oberfläche des Molybdäns.Are z. B. Mo rods immersed in the silicon-containing copper melt, the molybdenum on the surface becomes the dissolved silicon in molybdenum silicide converted while the copper does not react with the molybdenum. The ones from the melt removed molybdenum rods are then treated with dilute nitric acid, whereby the mechanically firmly adhering copper at the same time as that dissolved in the copper, Siliciam is not completely consumed for the build-up of the molybdenum silicide layer Will get removed. The molybdenum silicide layer is not attacked and remains as a uniformly thick, firmly adhering layer on the surface of the molybdenum.
Bei dem erfindungsgemäßen Verfahren wurde festgestellt, daß einwandfreie Silizierungsschichten in Kupferschmelzen mit einem Siliziumgehalt von 3 bis 30 0/0, vorzugsweise 10 bis 15 0%, bei Temperaturen von 800 bis 1200° C erhalten werden können. Es hat sich schließlich gezeigt, daß das Kupfer in der siliziumhaltigen Kupferschmelze noch bis zu 500/0 durch eines oder mehrere der anderen Metalle, wie Silber, Zinn, Zink, Blei, Kadmium, Gold, ersetzt werden kann, um vor allem den Schmelzpunkt der Schmelze herabzusetzen. Bei Ersatz des Siliziums bis zu etwa 2011/a durch Bor ist es möglich, in die Silizierungsschicht einen kleinen Gehalt von Bor einzubauen, was sich auf die Qualität der Silizierungsschicht in bezug auf Oxydationsbeständigkeit und Temperaturwechselbeständigkeit günstig auswirkt.In the method according to the invention it was found that perfect Silication layers in copper melts with a silicon content of 3 to 30 0/0, preferably 10 to 15 0%, at temperatures of 800 to 1200 ° C can be obtained can. It has finally been shown that the copper in the silicon-containing Copper melt still up to 500/0 through one or more of the other metals, such as Silver, tin, zinc, lead, cadmium, gold, can be replaced, especially to reduce the melting point reduce the melt. If the silicon is replaced by boron up to around 2011 / a it is possible to incorporate a small amount of boron into the siliconizing layer, which affects the quality of the siliconized layer in terms of resistance to oxidation and resistance to temperature changes has a beneficial effect.
Claims (5)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT1109482X | 1958-06-04 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1109482B true DE1109482B (en) | 1961-06-22 |
Family
ID=3685633
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEM41076A Pending DE1109482B (en) | 1958-06-04 | 1959-04-06 | Process for the production of siliconizing layers |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1109482B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1184595B (en) * | 1959-02-06 | 1964-12-31 | Plansee Metallwerk | Process for removing Si or Cr-containing copper layers |
| DE1289379B (en) * | 1962-10-16 | 1969-02-13 | North American Aviation Inc | Process for the production of chromium-containing coatings |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH310262A (en) * | 1951-06-29 | 1955-10-15 | Climax Molybdenum Co | Process for producing an oxidation-resistant coating on an object consisting of at least 50% molybdenum and object obtained by this process. |
-
1959
- 1959-04-06 DE DEM41076A patent/DE1109482B/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH310262A (en) * | 1951-06-29 | 1955-10-15 | Climax Molybdenum Co | Process for producing an oxidation-resistant coating on an object consisting of at least 50% molybdenum and object obtained by this process. |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1184595B (en) * | 1959-02-06 | 1964-12-31 | Plansee Metallwerk | Process for removing Si or Cr-containing copper layers |
| DE1289379B (en) * | 1962-10-16 | 1969-02-13 | North American Aviation Inc | Process for the production of chromium-containing coatings |
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