EP0281641B1 - Process for improving the corrosion resistance of hard or semi-hard copper fitting tubes - Google Patents
Process for improving the corrosion resistance of hard or semi-hard copper fitting tubes Download PDFInfo
- Publication number
- EP0281641B1 EP0281641B1 EP87103276A EP87103276A EP0281641B1 EP 0281641 B1 EP0281641 B1 EP 0281641B1 EP 87103276 A EP87103276 A EP 87103276A EP 87103276 A EP87103276 A EP 87103276A EP 0281641 B1 EP0281641 B1 EP 0281641B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- tubes
- hard
- heated
- corrosion resistance
- semi
- 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.)
- Expired
Links
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000010949 copper Substances 0.000 title claims abstract description 8
- 238000005260 corrosion Methods 0.000 title claims abstract description 8
- 230000007797 corrosion Effects 0.000 title claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 7
- 239000000314 lubricant Substances 0.000 claims abstract description 11
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 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
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 239000011135 tin Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 1
- 239000011133 lead Substances 0.000 claims 1
- 238000001953 recrystallisation Methods 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000013003 hot bending Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
Definitions
- the invention relates to a method according to the preamble of claim 1.
- Seamless drawn tubes made of phosphorus-deoxidized copper are produced as hard tube tubes and as soft-annealed tubes, especially coils, and are used extensively for the production of cold and hot water pipes in building construction.
- the invention is therefore based on the object of specifying a method for improving the corrosion resistance of hard or semi-hard pipes.
- the object is achieved in that the tubes for combustion of the lubricant residues are heated to a temperature which is below the lower limit of the recrystallization range for the tubes, an oxidizing atmosphere being present inside the tube.
- the temperature for the heating is selected in accordance with the softening curve for copper.
- the illustration shows the basic course of a softening curve (hardness as a function of temperature).
- the course of the curve is particularly dependent on the degree of drawing of the pipes and the duration of the heating. For example, as the degree of drawing increases, the start of recrystallization begins at lower temperatures.
- the pipes can be heated at higher temperatures if the pipes contain, according to the invention, additions of a maximum of 0.1% iron, cobalt, nickel, zinc, aluminum, lead, chromium, cadmium, magnesium, manganese, titanium, tin and / or zirconium (Specification in percent by weight).
- the tubes are heated at a take-off speed of 40 to 80 m / min.
- an oxygen-containing gas is preferably supplied to the interior of the tube in such an amount that it is sufficient for the complete combustion of the lubricant residues. It is recommended to introduce air or oxygen-enriched air into the inside of the pipe.
- Table II shows the strength values (Brinell hardness HB) and residue values measured on the pipes.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Heat Treatment Of Articles (AREA)
- Lubricants (AREA)
- Metal Extraction Processes (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Rigid Pipes And Flexible Pipes (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren nach dem Oberbegriff des Anspruchs 1.The invention relates to a method according to the preamble of claim 1.
Nahtlos gezogene Rohre aus phosphordesoxidiertem Kupfer werden als harte Stangenrohre und als weichgeglühte, insbesondere zu Ringen, gewickelte Rohre produziert und in großem Umfang für die Herstellung von Kalt- und Warmwasserleitungen im Hochbau verwendet.Seamless drawn tubes made of phosphorus-deoxidized copper are produced as hard tube tubes and as soft-annealed tubes, especially coils, and are used extensively for the production of cold and hot water pipes in building construction.
Die Erfahrung hat gezeigt, daß die Korrosionsbeständigkeit der Rohre wesentlich verbessert wird, wenn die vom Rohrziehen stammenden Schmiermittelrückstände weitgehend entfernt werden.Experience has shown that the corrosion resistance of the pipes is significantly improved if the lubricant residues from pipe drawing are largely removed.
Bei weichgeglühten Rohren sind hierfür eine Reihe von Verfahren bekanntgeworden (vgl. beispielsweise DE-PS 3.003.228).In the case of soft annealed tubes, a number of methods have become known for this (see, for example, DE-PS 3,003,228).
Bei harten Rohren hat man bisher versucht, den Schmiermittelfilm durch Lösungsmittelbehandlung zu entfernen. Diese Behandlung war allerdings nicht ausreichend; denn bei einer Wärmebehandlung der Rohre auf der Baustelle, insbesondere beim Hartlöten oder Warmbiegen, treten an den behandelten Stellen gelegentlich Korrosionserscheinungen auf, wenn die Qualität des Wassers dementsprechend ist.So far, attempts have been made to remove the lubricant film by means of solvent treatment in the case of hard pipes. However, this treatment was not sufficient; Because with heat treatment of the pipes on the construction site, especially when brazing or hot bending, the treated places occasionally show signs of corrosion if the quality of the water is corresponding.
Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren zur Verbesserung der Korrosionsbeständigkeit von harten bzw. halbharten Rohren anzugeben.The invention is therefore based on the object of specifying a method for improving the corrosion resistance of hard or semi-hard pipes.
Die Aufgabe wird erfindungsgemäß dadurch gelöst, daß die Rohre zur Verbrennung der Schmiermittelrückstände maximal auf eine Temperatur erwärmt werden, die unterhalb der unteren Grenze des Rekristallisationsbereichs für die Rohre liegt, wobei im Rohrinneren eine oxidierende Atmosphäre vorliegt.The object is achieved in that the tubes for combustion of the lubricant residues are heated to a temperature which is below the lower limit of the recrystallization range for the tubes, an oxidizing atmosphere being present inside the tube.
Es hat sich überraschend gezeigt, daß mit dieser Erwärmung der harten bzw. halbharten Rohre eine Verbrennung des Schmiermittelfilms möglich ist und gleichzeitig ein ausreichender Kupferoxidfilm (Cu20) erzielt wird, der zur Verhinderung der Korrosion beiträgt. Die Rohre sind also auf eine Temperatur zu erwärmen, die mindestens so hoch ist, daß eine Verbrennung der Schmiermittelrückstände möglich ist, und die andererseits unterhalb der unteren Grenze des Rekristallisationsbereichs liegt.It has surprisingly been found that with this heating of the hard or semi-hard pipes, combustion of the lubricant film is possible and, at the same time, a sufficient copper oxide film (Cu 2 O) is achieved which contributes to the prevention of corrosion. The pipes must therefore be heated to a temperature which is at least high enough to allow combustion of the lubricant residues and which is below the lower limit of the recrystallization range.
Nach einer besonderen Ausführungsform der Erfindung wird die Temperatur für die Erwärmung entsprechend der Entfestigungskurve für Kupfer gewählt. Zur Erläuterung ist in der Abbildung der prinzipielle Verlauf einer Entfestigungskurve (Härte als Funktion der Temperatur) dargestellt. Der Rekristallisationsbereich setzt - wie allgemein bekannt - zu Beginn des Steilabfalls der Kurve ein (= untere Grenze des Rekristallisationsbereichs). Der Verlauf der Kurve ist insbesondere stark abhängig vom Ziehgrad der Rohre und von der Dauer der Erwärmung. So setzt beispielsweise bei zunehmendem Ziehgrad der Beginn der Rekristallisation bereits bei niedrigeren Temperaturen ein.According to a particular embodiment of the invention, the temperature for the heating is selected in accordance with the softening curve for copper. The illustration shows the basic course of a softening curve (hardness as a function of temperature). The recrystallization area begins - as is generally known - at the beginning of the steep decline of the curve (= lower limit of the recrystallization area). The course of the curve is particularly dependent on the degree of drawing of the pipes and the duration of the heating. For example, as the degree of drawing increases, the start of recrystallization begins at lower temperatures.
Durch die Wahl der Maximaltemperatur unterhalb der unteren Grenze des Rekristallisationsbereichs ist also sichergestellt, daß der harte bzw. halbharte Zustand der Rohre erhalten bleibt.The choice of the maximum temperature below the lower limit of the recrystallization range ensures that the hard or semi-hard condition of the tubes is maintained.
Es empfiehlt sich, die Rohre auf 250 - 350 0 C zu erwärmen.It is advisable to heat the pipes to 250 - 350 0 C.
Die Erwärmung der Rohre kann bei höheren Temperaturen erfolgen, sofern die Rohre erfindungsgemäß Zusätze von insgesamt maximal 0,1 % Eisen, Kobalt, Nickel, Zink, Aluminium, Blei, Chrom, Kadmium, Magnesium, Mangan, Titan, Zinn und/oder Zirkon enthalten (Angabe in Gewichtsprozent).The pipes can be heated at higher temperatures if the pipes contain, according to the invention, additions of a maximum of 0.1% iron, cobalt, nickel, zinc, aluminum, lead, chromium, cadmium, magnesium, manganese, titanium, tin and / or zirconium (Specification in percent by weight).
Durch diese Zusätze wird die untere Grenze des Rekristallisationsbereichs zu höheren Temperaturen verschoben, d.h., es ist eine beschleunigte Verbrennung des Schmiermittelfilms bei höheren Temperaturen möglich, ohne daß ein Härteverlust eintritt. Durch diese Zusätze werden Temperaturerhöhungen von etwa 30 - 40 0 C ermöglicht.These additives shift the lower limit of the recrystallization range to higher temperatures, i.e. accelerated combustion of the lubricant film at higher temperatures is possible without loss of hardness. These additives enable temperature increases of approximately 30-40 ° C.
Nach einer besonderen Ausführungsform der Erfindung werden die Rohre bei einer Abzugsgeschwindigkeit von 40 bis 80 m/min erwärmt.According to a special embodiment of the invention, the tubes are heated at a take-off speed of 40 to 80 m / min.
Sofern die Erwärmung bei ruhender Luft nicht ausreichend ist, wird dem Rohrinneren vorzugsweise ein sauerstoffhaltiges Gas in einer solchen Menge zugeführt, daß sie zur vollständigen Verbrennung der Schmiermittelrückstände ausreicht. Dabei empfiehlt es sich, Luft oder mit Sauerstoff angereicherte Luft in das Rohrinnere einzuleiten.If the heating is not sufficient when the air is still, an oxygen-containing gas is preferably supplied to the interior of the tube in such an amount that it is sufficient for the complete combustion of the lubricant residues. It is recommended to introduce air or oxygen-enriched air into the inside of the pipe.
Die Erfindung wird anhand der folgenden Ausführungsbeispiele näher erläutert:The invention is explained in more detail using the following exemplary embodiments:
Zur Untersuchung standen sechs auf die Endabmessung 15 x 1 mm gezogene Rohre aus phosphordesoxidiertem Kupfer in Form von Großringen der Länge 650 m zur Verfügung. Die Rohre mit einem Rest-Schmiermittelgehalt von 0,06 bis 0,08 mg C/dm2 wurden mit einer Abzugsgeschwindigkeit von 50 m/min durch eine Strecke zur Widerstandserwärmung geführt und auf die Temperaturen gemäß folgender Tabelle I erwärmt. Die Erwärmung erfolgte bei Luft bzw. nach der Auffüllung der Großringe mit einem Sauerstoff/Stickstoff-Gemisch 50 % 02/50 % N2.
In der Tabelle II sind die an den Rohren gemessenen Festigkeitswerte (Brinell-Härte HB) und Rückstandswerte aufgeführt.
Es zeigt sich, daß bei der durchgeführten Erwärmung der Rohre nicht nur der harte bzw. halbharte Zustand der Rohre erhalten bleibt, sondern auch der Restkohlenstoffgehalt unter der üblicherweise geforderten Grenze von 0,06 mg C/dm2 liegt. An den untersuchten Rohren wurden außerdem dünne Oxidfilme (CU20) festgestellt, die ebenfalls für eine gute Korrosionsbeständigkeit verantwortlich sind.It turns out that when the pipes are heated, not only the hard or semi-hard condition of the pipes is preserved, but also the residual carbon content is below the limit of 0.06 mg C / dm 2 that is usually required. Thin oxide films (C U2 0) were also found on the pipes examined, which are also responsible for good corrosion resistance.
Claims (8)
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE8787103276T DE3760510D1 (en) | 1987-03-07 | 1987-03-07 | Process for improving the corrosion resistance of hard or semi-hard copper fitting tubes |
| AT87103276T ATE45993T1 (en) | 1987-03-07 | 1987-03-07 | METHOD OF IMPROVING THE CORROSION RESISTANCE OF HARD SEMI-HARD COPPER INSTALLATION TUBES. |
| EP87103276A EP0281641B1 (en) | 1987-03-07 | 1987-03-07 | Process for improving the corrosion resistance of hard or semi-hard copper fitting tubes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP87103276A EP0281641B1 (en) | 1987-03-07 | 1987-03-07 | Process for improving the corrosion resistance of hard or semi-hard copper fitting tubes |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0281641A1 EP0281641A1 (en) | 1988-09-14 |
| EP0281641B1 true EP0281641B1 (en) | 1989-08-30 |
Family
ID=8196808
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP87103276A Expired EP0281641B1 (en) | 1987-03-07 | 1987-03-07 | Process for improving the corrosion resistance of hard or semi-hard copper fitting tubes |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0281641B1 (en) |
| AT (1) | ATE45993T1 (en) |
| DE (1) | DE3760510D1 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3827353A1 (en) * | 1988-08-12 | 1990-02-22 | Kabelmetal Ag | INTERNAL OXIDIZED TUBES |
| DE4334536A1 (en) * | 1993-10-09 | 1995-04-13 | Kabelmetal Ag | Process for the production of seamless drawn semi-hard / hard installation pipes |
| FI107543B (en) | 1998-07-30 | 2001-08-31 | Outokumpu Oy | Process for making a copper tube |
| FI120359B (en) * | 2002-12-18 | 2009-09-30 | Cupori Group Oy | Method and apparatus for treating an inner surface of a copper or copper alloy tube |
| DE102007055446A1 (en) * | 2007-11-12 | 2009-05-14 | Hansgrohe Ag | Provision of water-bearing components from brass alloys with reduced metal ion release |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| LU67959A1 (en) * | 1973-07-06 | 1975-04-11 | ||
| FR2308436A1 (en) * | 1975-04-25 | 1976-11-19 | Cit Alcatel | TREATMENT OF COPPER AND ALLOY TUBES FOR THE ELIMINATION OF CARBON PRODUCTS EXISTING FROM THEIR SURFACE |
| DE2928084C2 (en) * | 1979-07-12 | 1987-01-02 | Kabel- und Metallwerke Gutehoffnungshütte AG, 3000 Hannover | Process for treating copper pipes |
| DE3003228C2 (en) | 1980-01-30 | 1981-11-26 | Wieland-Werke Ag, 7900 Ulm | Process for improving the corrosion resistance of installation pipes made of copper |
-
1987
- 1987-03-07 DE DE8787103276T patent/DE3760510D1/en not_active Expired
- 1987-03-07 EP EP87103276A patent/EP0281641B1/en not_active Expired
- 1987-03-07 AT AT87103276T patent/ATE45993T1/en active
Also Published As
| Publication number | Publication date |
|---|---|
| EP0281641A1 (en) | 1988-09-14 |
| DE3760510D1 (en) | 1989-10-05 |
| ATE45993T1 (en) | 1989-09-15 |
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