US3729308A - Iron nickel chromium alloys - Google Patents
Iron nickel chromium alloys Download PDFInfo
- Publication number
- US3729308A US3729308A US00056977A US3729308DA US3729308A US 3729308 A US3729308 A US 3729308A US 00056977 A US00056977 A US 00056977A US 3729308D A US3729308D A US 3729308DA US 3729308 A US3729308 A US 3729308A
- Authority
- US
- United States
- Prior art keywords
- percent
- alloys
- alloy
- resistance
- oxidation
- 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 - Lifetime
Links
- 239000000788 chromium alloy Substances 0.000 title description 3
- BIJOYKCOMBZXAE-UHFFFAOYSA-N chromium iron nickel Chemical compound [Cr].[Fe].[Ni] BIJOYKCOMBZXAE-UHFFFAOYSA-N 0.000 title description 3
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 title description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 69
- 239000000956 alloy Substances 0.000 abstract description 69
- 230000003647 oxidation Effects 0.000 abstract description 35
- 238000007254 oxidation reaction Methods 0.000 abstract description 35
- 239000011651 chromium Substances 0.000 abstract description 33
- 238000005260 corrosion Methods 0.000 abstract description 29
- 230000007797 corrosion Effects 0.000 abstract description 27
- 229910052684 Cerium Inorganic materials 0.000 abstract description 24
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract description 24
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052804 chromium Inorganic materials 0.000 abstract description 20
- 229910052710 silicon Inorganic materials 0.000 abstract description 20
- 239000010703 silicon Substances 0.000 abstract description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 48
- 229910052759 nickel Inorganic materials 0.000 description 20
- 238000005336 cracking Methods 0.000 description 18
- 239000011572 manganese Substances 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 125000004122 cyclic group Chemical group 0.000 description 12
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 9
- 229910052748 manganese Inorganic materials 0.000 description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 239000010936 titanium Substances 0.000 description 8
- 229910052719 titanium Inorganic materials 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000004580 weight loss Effects 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 230000002411 adverse Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 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 description 4
- 229910001122 Mischmetal Inorganic materials 0.000 description 3
- 238000007792 addition Methods 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 230000001747 exhibiting effect Effects 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
- 230000002459 sustained effect Effects 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- -1 particularly Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C1/00—Details
- H01C1/02—Housing; Enclosing; Embedding; Filling the housing or enclosure
- H01C1/028—Housing; Enclosing; Embedding; Filling the housing or enclosure the resistive element being embedded in insulation with outer enclosing sheath
Definitions
- Iron-base alloys for sheathing electric heater elements include specially proportioned amounts of nickel (about to about 23%), chromium (about 17% to about 23%), silicon (about 0.3% to about 1.5%) and cerium (an effective amount up to about .05%) to assure high oxidation resistance and good corrosion resistance.
- This invention is directed to improved oxidation and corrosion resistant low cost iron-base alloys particularly suitable for use as electric heater element sheathing.
- One type of electric heater element comprises a resistance conductor which is enclosed in a tubular metal sheath, with the resistance conductor embedded in and supported in spaced relation to the sheath by a densely compacted layer of refractory, heat-conducting, electrically insulating material.
- the resistance conductor may be a helically wound wire member and the refractory insulating material may be granular magnesium oxide (Ma A commercial alloy which is currently used as sheathing material is an iron-base alloy which nominally contains, by weight, 32.5% nickel, 21% chromium, and small amounts of carbon, manganese, sulfur, silicon, copper, aluminum and titanium.
- the present invention contemplates weldable iron-base alloys composed of, by weight, from about 15% to about 23% nickel, from about 17% to about 23% chromium, from about 0.3% to about 1.5% silicon, cerium in a small but effective amount sufiicient to improve oxidation and corrosion resistance, the cerium being up to about 0.05%, up to about 2% manganese, up to about 0.15% carbon, up to about 0.5% aluminum,
- these elements should be controlled such that the ratio percent Mn/ (percent Si-i-percent Ce) has a value less than about 0.6 and the ratio percent Ni/ percent Cr has a value in the range from 0.9 to 1.2.
- the alloys of the invention exhibit resistance to cyclic oxidation at 1800 F. equal to or superior to that of the sheathing alloys commonly used.
- An advantageous composition of the alloy of the invention is composed of, by weight, about 20% nickel, about 20% chromium, about 0.6% silicon, about 0.02% cerium and the balance essentially iron except for small amounts of incidental elements and impurities including up to about 1% manganese.
- chromium and nickel promote resistance to oxidation, as well as resistance to general corrosion and to stress corrosion. Chromium in amounts in excess of about 23% has an adverse effect on workability. In general, the higher the chromium content within the specified range, the better the alloy produced, particularly with respect to oxidation resistance. Amounts of nickel beyond 23% are unnecessary and should the percentage fall much below 15% various characteristics can be adversely affected. In seeking the best combination of results a range of from 19% to 21% or 22% chromium and from about 18% to 22.5% nickel is quite satisfactory.
- Cerium is advantageously present in the alloys in the amount of from about 0.01% to about 0.05%. The element cerium in amounts Within the specified range makes an important contribution to the oxidation resistance and to stress corrosion resistance. It is good practice to include at least 0.01% cerium since the alloys are then less sensitive in respect of their corrosion resistance to variations in the amounts of the other alloy constituents, particularly, nickel, chromium, silicon and manganese. Quantities of cerium in excess of the specified range lead to difficulties in forging, rolling and in weldability. Thus, a cerium range of from 0.015% to about 0.04% is preferred.
- cerium which is employed in the alloys of this invention is ordinarily added as misch metal which also contains lanthanum and other rare earth elements.
- misch metal which also contains lanthanum and other rare earth elements.
- an addition of misch metal is composed, by weight,
- the alloys of the invention may also include relatively small amounts of other elements which can be present as impurities without substantial detrimental effect. Such elements are contained in the alloys of the invention due to their unavoidable presence in the raw materials employed, or as a result of their use for one purpose or another during the preparation of the alloys. Thus, manganese in the amount of up to 2%, by weight, may be tolerated, but it is more advantageous to have no more than 1% present. Manganese in amounts in excess of the specified maximum has an adverse effect upon oxidation resistance and upon stress corrosion cracking. Up to about 0.15% by weight of carbon can be tolerated, but it is desirable that the alloy contain no more than about 0.1%.
- EXAMPLE A number of heats of the alloys of the invention were prepared by charging appropriate amounts of iron, nickel and chromium into an air induction furnace and melting down the charge. Just before tapping the heat, the required silicon, aluminum, titanium and cerium additions (the latter in the form of misch metal) were added, and last of all, calcium. The heat was then poured into molds to produce 4 inch diameter ingots. The ingots thus prepared were forged into A-inch thick flat bars and then the fiat bars were cold rolled to 0.125 inch thick sheet.
- Sections were cut from the sheet for use as cyclic oxidation specimens and for standard U-bend stress corrosion cracking test specimens and the remaining sections of the sheet were then welded end to end to make a roll of sheet which was then cold rolled to 0.025 inch thick sheet, the gauge commonly employed in making heater element sheathing.
- Table I gives the composition of abnumber of alloys which were prepared as described a ove.
- the ratio of nickel to chromium be at least unity, the silicon content should be 1% or more and the manganese should not exceed 0.5
- the alloys of Table I were further tested for weldability by preparing autogenous TIG Welds and examining the welds for cracking.
- the weldability of the alloys ranged from good to excellent.
- the alloys of the present invention also exhibit a resistance to general corrosion similar to that of Type 304 stainless steel. This property is of some importance in view of the fact that in normal use as sheathing alloys, they are often exposed to contact with various solutions at elevated temperature.
- a weldable, oxidation and corrosion-resistant alloy consisting essentially, by weight, of from about 15% to about 23% nickel, from about 17% to about 23% chromium, from about 0.3% to about 1.5% silicon, from a small but effective amount of cerium up to about 0.05 to improve oxidation and corrosion resistance, up to about 2 manganese, up to about 0.15% carbon, up to about 0.5% aluminum, up to about 0.5 titanium, up to about 0.015% sulfur and the balance essentially iron, which is characterized by exhibiting high resistance to cyclic oxidation resulting from balancing the constituents of the alloy within the ranges stated according to the following formula:
- the alloy of claim 1 containing from 18% to 22.5% nickel, from 19% to 22% chromium, from about 0.6% to about 1.1% silicon and from 0.015% to about 0.04% cerium.
- the alloy of claim 2 wherein nickel is present in the amount of about 20, the chromium is present in the amount of about 20% 6.
- the alloy of claim 3 wherein nickel is present in the amount of about 20%, and chromium is present in the amount of about 20% 7.
- the alloy of claim 1 wherein the nickel is present in the amount of about 20%, chromium is present in the amount of about 20%, silicon is present in the amount of at least about 0.6% and cerium is present in the amount of about 0.02%
- a weldable, oxidation and corrosion-resistant alloy consisting essentially by weight, of from about 15% to about 23% nickel, from about 17% to about 23% chromium, from about 0.3% to about 1.5% silicon, from a small but effective amount of cerium up to about 0.05% to improve oxidation and corrosion resistance, up to about 2% manganese, up to about 0.15 carbon, up to about 0.5 aluminum, up to about 0.5% titanium, up to about 0.015% sulfur and the balance essentially iron, which is characterized by exhibiting high resistance to cyclic oxidation resulting from balancing the constituents of the alloy within the ranges stated according to the following formula:
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Resistance Heating (AREA)
- Heat Treatment Of Steel (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US5697770A | 1970-07-21 | 1970-07-21 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3729308A true US3729308A (en) | 1973-04-24 |
Family
ID=22007746
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00056977A Expired - Lifetime US3729308A (en) | 1970-07-21 | 1970-07-21 | Iron nickel chromium alloys |
Country Status (12)
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4007038A (en) * | 1975-04-25 | 1977-02-08 | Allegheny Ludlum Industries, Inc. | Pitting resistant stainless steel alloy having improved hot-working characteristics |
| US4043838A (en) * | 1975-04-25 | 1977-08-23 | Allegheny Ludlum Industries, Inc. | Method of producing pitting resistant, hot-workable austenitic stainless steel |
| US4063935A (en) * | 1973-12-22 | 1977-12-20 | Nisshin Steel Co., Ltd. | Oxidation-resisting austenitic stainless steel |
| US4102225A (en) * | 1976-11-17 | 1978-07-25 | The International Nickel Company, Inc. | Low chromium oxidation resistant austenitic stainless steel |
| US4293335A (en) * | 1977-12-08 | 1981-10-06 | Asahi Glass Company, Ltd. | Roll for manufacturing float glass |
| US4950873A (en) * | 1984-04-27 | 1990-08-21 | Sumitomo Metal Industries, Ltd. | Sheath heater |
| US4999158A (en) * | 1986-12-03 | 1991-03-12 | Chrysler Corporation | Oxidation resistant iron base alloy compositions |
| US5160382A (en) * | 1992-01-17 | 1992-11-03 | Inco Alloys International, Inc. | Heater sheath alloy |
| US5217545A (en) * | 1992-01-17 | 1993-06-08 | Inco Alloys International, Inc. | Heater sheath alloy |
| EP3467137A4 (en) * | 2016-05-31 | 2019-11-20 | Nippon Yakin Kogyo Co., Ltd. | FE-NI-CR ALLOY, FE-NI-CR ALLOY STRIP, METHOD FOR PRODUCING A FE-NI-CR ALLOY AND METHOD FOR PRODUCING A SLEEVE HEATER |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5114118A (en) * | 1974-07-25 | 1976-02-04 | Nisshin Steel Co Ltd | Oosutenaitokeitainetsuko |
| SE419102C (sv) | 1974-08-26 | 1985-12-23 | Avesta Ab | Anvendning av ett kromnickelstal med austenitisk struktur till konstruktioner som erfordrar hog extrem krypbestendighet vid konstant temperatur upp till 1200?59c |
-
1970
- 1970-07-21 US US00056977A patent/US3729308A/en not_active Expired - Lifetime
-
1971
- 1971-06-09 CA CA115,243A patent/CA947119A/en not_active Expired
- 1971-06-25 ZA ZA714178A patent/ZA714178B/xx unknown
- 1971-07-06 GB GB3172571A patent/GB1316048A/en not_active Expired
- 1971-07-14 NL NL717109700A patent/NL148359B/xx unknown
- 1971-07-20 DE DE19712136177 patent/DE2136177A1/de active Pending
- 1971-07-20 NO NO712771A patent/NO129097B/no unknown
- 1971-07-20 FR FR7126449A patent/FR2099329A5/fr not_active Expired
- 1971-07-20 CH CH1070371A patent/CH542285A/fr not_active IP Right Cessation
- 1971-07-20 SE SE7109321A patent/SE377137B/xx unknown
- 1971-07-20 BE BE770263A patent/BE770263A/xx unknown
- 1971-07-20 JP JP5366971A patent/JPS5529146B1/ja active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4063935A (en) * | 1973-12-22 | 1977-12-20 | Nisshin Steel Co., Ltd. | Oxidation-resisting austenitic stainless steel |
| US4108641A (en) * | 1973-12-22 | 1978-08-22 | Nisshin Steel Company, Limited | Oxidation-resisting austenitic stainless steel |
| US4007038A (en) * | 1975-04-25 | 1977-02-08 | Allegheny Ludlum Industries, Inc. | Pitting resistant stainless steel alloy having improved hot-working characteristics |
| US4043838A (en) * | 1975-04-25 | 1977-08-23 | Allegheny Ludlum Industries, Inc. | Method of producing pitting resistant, hot-workable austenitic stainless steel |
| US4102225A (en) * | 1976-11-17 | 1978-07-25 | The International Nickel Company, Inc. | Low chromium oxidation resistant austenitic stainless steel |
| US4293335A (en) * | 1977-12-08 | 1981-10-06 | Asahi Glass Company, Ltd. | Roll for manufacturing float glass |
| US4950873A (en) * | 1984-04-27 | 1990-08-21 | Sumitomo Metal Industries, Ltd. | Sheath heater |
| US4999158A (en) * | 1986-12-03 | 1991-03-12 | Chrysler Corporation | Oxidation resistant iron base alloy compositions |
| US5160382A (en) * | 1992-01-17 | 1992-11-03 | Inco Alloys International, Inc. | Heater sheath alloy |
| US5217545A (en) * | 1992-01-17 | 1993-06-08 | Inco Alloys International, Inc. | Heater sheath alloy |
| EP3467137A4 (en) * | 2016-05-31 | 2019-11-20 | Nippon Yakin Kogyo Co., Ltd. | FE-NI-CR ALLOY, FE-NI-CR ALLOY STRIP, METHOD FOR PRODUCING A FE-NI-CR ALLOY AND METHOD FOR PRODUCING A SLEEVE HEATER |
| US10927438B2 (en) | 2016-05-31 | 2021-02-23 | Nippon Yakin Kogyo Co., Ltd. | Fe-Ni-Cr alloy, Fe-Ni-Cr alloy strip, sheath heater, method of manufacturing Fe-Ni-Cr alloy, and method of manufacturing sheath heater |
Also Published As
| Publication number | Publication date |
|---|---|
| NO129097B (enrdf_load_stackoverflow) | 1974-02-25 |
| FR2099329A5 (enrdf_load_stackoverflow) | 1972-03-10 |
| CH542285A (fr) | 1973-09-30 |
| DE2136177A1 (de) | 1972-03-09 |
| JPS5529146B1 (enrdf_load_stackoverflow) | 1980-08-01 |
| CA947119A (en) | 1974-05-14 |
| ZA714178B (en) | 1972-03-29 |
| NL7109700A (enrdf_load_stackoverflow) | 1972-01-25 |
| AU3144671A (en) | 1973-01-25 |
| GB1316048A (en) | 1973-05-09 |
| NL148359B (nl) | 1976-01-15 |
| SE377137B (enrdf_load_stackoverflow) | 1975-06-23 |
| BE770263A (fr) | 1972-01-20 |
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