SE454889B - PROCEDURE FOR CONTINUOUS GLODGA ZIRCONIUM - Google Patents

PROCEDURE FOR CONTINUOUS GLODGA ZIRCONIUM

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Publication number
SE454889B
SE454889B SE8105889A SE8105889A SE454889B SE 454889 B SE454889 B SE 454889B SE 8105889 A SE8105889 A SE 8105889A SE 8105889 A SE8105889 A SE 8105889A SE 454889 B SE454889 B SE 454889B
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Sweden
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trans
nitrogen
zirconium
annealing
long
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SE8105889A
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Swedish (sv)
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SE8105889L (en
Inventor
M E Craig
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Teledyne Ind
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Application filed by Teledyne Ind filed Critical Teledyne Ind
Publication of SE8105889L publication Critical patent/SE8105889L/en
Publication of SE454889B publication Critical patent/SE454889B/en

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    • 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
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium 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
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Heat Treatment Of Nonferrous Metals Or Alloys (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)
  • Fertilizers (AREA)

Description

454 889 ter. Det har vidare befunnits att reaktionen mellan metallen och kväve är tillräckligt långsam för att inte bara göra denna glödg- ning i kväveatmosfär möjlig utan även önskvärd. Glëdgningsprocessen v i kväve enligt föreliggande uppfinning ger en mindre kornstorleks- tillväxt på grund av den begränsade utsättningen för värme. Denna finare kornstorlek ger upphov till ökad sträckgräns och dragbrott- hållfasthet. 454 889 ter. It has further been found that the reaction between the metal and nitrogen is slow enough to not only make this annealing in a nitrogen atmosphere possible but also desirable. The nitrogen v-annealing process of the present invention results in smaller grain size growth due to the limited exposure to heat. This finer grain size gives rise to an increased yield strength and tensile strength.

Denna glödgningsprocess i kväve är även mycket mer ekonomisk än* glödgníng i vakuum därigenom att produkten framställes mycket snab- bare, apparaturen för kontinuerlig glödgning är mindre kostsam än för glödgning i vakuum, och produktionskostnaden för underhållande av en kväveatmosfär kontra en vakuumatmosfär är väsentligt lägre.This annealing process in nitrogen is also much more economical than * annealing in vacuum in that the product is produced much faster, the apparatus for continuous annealing is less expensive than for annealing in vacuum, and the production cost for maintaining a nitrogen atmosphere versus a vacuum atmosphere is significantly lower.

Följande exempel gjordes och testades med avseende på hållfasthet och formbarhet, och resultaten är illustrerade i de tabeller som åter- ges nedan. Ett band Zircaloy-4 med följande analys framställdes på följande sätt: Zircalo - nominellt 15% sn 0,273 Fe o,1% o: rest Zr ' Detta material framställdes genom varmsmíde i betafas, varmvalsning i alfafas och kallvalsning med åtminstone 50% reduktion med mellan- glödgningar i alfafas följande vardera 30-40% reduktion.The following examples were made and tested for strength and formability, and the results are illustrated in the tables set forth below. A strip of Zircaloy-4 with the following analysis was prepared as follows: Zircalo - nominal 15% sn 0.273 Fe o, 1% o: residue Zr 'This material was prepared by hot forging in beta phase, hot rolling in alpha phase and cold rolling with at least 50% reduction with between - alpha phase annealing following a 30-40% reduction each.

Legeringen behandlades med Slödëniflš i Vakuum °°h i kväve och testades sedan med avseende på sträckgräns, dragbrotthållfasthet, töjning, formbarhet, och slutligen upptagning av kväve och syre. 454 889 Resultaten av dessa tester framställs i följande tabeller.The alloy was treated with Slödëni fl š in Vacuum °° h in nitrogen and then tested for tensile strength, tensile strength, elongation, formability, and finally nitrogen and oxygen uptake. 454,889 The results of these tests are presented in the following tables.

Den ovan nämnda zirkoniumlegeringen under 3 minuter via 7oo°c (13oo°F>¿ Den testades seaen både i war- led och i längdled med avseende på förlängning, dragbrotthållfast- ,glödgades i kväve het och sträckgräns. Resultaten redovisas i tabell I.The above-mentioned zirconium alloy for 3 minutes via 70 ° C (130 ° F> ¿The sea was tested both vertically and longitudinally with respect to elongation, tensile strength, annealed in nitrogen and yield strength. The results are reported in Table I.

TABELL I Dragbrott- Sträck- hàllšasthet gräns Exempel % töjning N/mm N/mm Zr~4, Trans. 32 446 352 " ", Trans. 31 446 350 " ", Trans. 32 437 340 " " Long. 32 440 328 " ", Long. 31 438 330 " ", Long. 31 440 335 Trans. = transversell testning Long. = longitudinell testning "En jämförelse gjordes mellan genomsnittet av resultaten i tabell I och samma legering behandlad med glödgning i vakuum. Denna jäm- förelse visas i följande tabell II som också visar en jämförelse av kornstorlekar. 454 889 4 TABELL II in: Dragbrott- Sträck- Kornstorlek n hàllšasthet gränâ (Kornsumflßkstal Exempel % töjning N/mm N/mm enligt ASIM speci- fikation E112) 7. zr-4, long. 34 418 337 9-1/2 8. " ", Trans. 34 417 340 9. " 'H long 31 402 392 10 10. " Trans. 32 410 332 ““ 11.* " ", Long. 31.3 439 331 10-1/2 31.7 443 348 12. * " ", Trans.TABLE I tensile strength - tensile strength limit Example% elongation N / mm N / mm Zr ~ 4, Trans. 32 446 352 "", Trans. 31 446 350 "", Trans. 32 437 340 "" Long. 32 440 328 "", Long. 31 438 330 "", Long. 31 440 335 Trans. = transverse testing Long. = longitudinal testing "A comparison was made between the average of the results in Table I and the same alloy treated with annealing in vacuum. This comparison is shown in the following Table II which also shows a comparison of grain sizes. 454 889 - Grain size n strength gränâ (Grain sum ß ßkstal Example% elongation N / mm N / mm according to ASIM specification E112) 7. zr-4, long. 34 418 337 9-1 / 2 8. "", Trans. 34 417 340 9 . "'H long 31 402 392 10 10." Trans. 32 410 332 ““ 11. * "", Long. 31.3 439 331 10-1 / 2 31.7 443 348 12. * "", Trans.

X- Glödgad i kväveatmosfär under 3 minuter vid 700°C (1 300°F).X- Annealed in a nitrogen atmosphere for 3 minutes at 700 ° C (1,300 ° F).

I tabell II glödgades 7-10 i vakuum och kan jämföras med exemplen 11-12, vilka har glödgats i kväve såsom ovan framställts.In Table II, 7-10 were annealed in vacuo and can be compared with Examples 11-12, which have been annealed in nitrogen as prepared above.

HIS '4s4 ss9 5 TABELL III Dragbrott- . ' hâllfast Sträck- Exempel Temp. % töjning het N/mm gräns N/mm 25.* zr-4 , Trans. ' 315°c 42 214 143 26.* H " , Trans. « 1- 43 214 141 27.* " " , Trans. " 41 215 145 28.- ~ -- , rang. -- 46 243 126 29.* " " , Long. " 46 V 244 128 30.* " " , rang. 1' "' 46 243 J 126 '3l. " " , Trans. " 43 ï35 121 32. " " , Trans. " 43 186 121 33. " “ , Trama. " 44 188 121 34. " " , long. " 51 202 114 35- " ". Lene- “ 51' zos 110 36. " ~', rang. " 52 ' 199 1oe 37.* " " , frrana. Rxr. 31 479 422 38.* " " , Trans. I" 31 474 421 39.* “ “ , Trans. " 31 ~ 477 418 40,* ß 1' , mng, " 32 503 353 41.* “ " , rang. " 26 sos 351 42.* " " , Lang. " _ 29 511 353 43. 1' -- , name. -- 3o 452 .B88 44. " " , Trans. “ 31 ' . 451 386 45. “ " , Trans. " 31 449 390 46. " " , Long. " 32 480 341 47. " " , mg. " 31 478 341 48. " " , Lang. " 30 484 349 * e1aagaa 1 kväve under 5 minuter vid 7oo°c <13oo°F1.HIS '4s4 ss9 5 TABLE III Traction break-. 'Durable Stretch- Example Temp. % elongation hot N / mm limit N / mm 25. * zr-4, Trans. '315 ° c 42 214 143 26. * H ", Trans.« 1- 43 214 141 27. * "", Trans. "41 215 145 28.- ~ -, rang. - 46 243 126 29. * "", Long. "46 V 244 128 30. *" ", rang. 1 '"' 46 243 J 126 '3l. "", Trans. "43 ï35 121 32." ", Trans." 43 186 121 33. "", Trama. "44 188 121 34." ", long. "51 202 114 35-" ". Lene-" 51 'zos 110 36. "~', rang. "52 '199 1oe 37. *" ", frrana. Rxr. 31 479 422 38. *" ", Trans. I" 31 474 421 39. * ““, Trans. "31 ~ 477 418 40, * ß 1 ', mng," 32 503 353 41. * “", rang. "26 sos 351 42. *" ", Lang. "_ 29 511 353 43. 1 '-, name. - 3o 452 .B88 44." ", Trans.“ 31'. 451 386 45. “", Trans. "31 449 390 46." ", Long." 32 480 341 47. "", mg. "31 478 341 48." ", Lang." 30 484 349 * e1aagaa 1 nitrogen for 5 minutes at 70 ° C <130 ° F1.

R.T. = rumstemperatur "Tabell III illuštrerar vidare på ett jämförande sätt egenskaper hos Zircaloy-4-metall, som har glödgats i kväve jämförd med samma Zirca- , loy-4-metall som har glödgats i vakuum.R.T. = room temperature "Table III further illustrates in a comparative manner the properties of Zircaloy-4 metal which has been annealed in nitrogen compared to the same Zirca-loy-4 metal which has been annealed in vacuum.

Två band Zircaloy-4 behandlades separat medelst glödgning i kväve _ och glödgning i vakuum och testades sedan med avseende på tänjbarhet och töjbarhet. Resultatet av detta prov återges i tabell IV där 2T och 1,6T representerar böjning av metallen kring en dorn med en radie 454 889 fr) som är två gånger respektive 1,6 gånger materialets tjocklek.Two Zircaloy-4 bands were treated separately by nitrogen annealing and vacuum annealing and then tested for extensibility and extensibility. The result of this test is given in Table IV where 2T and 1.6T represent the bending of the metal around a mandrel with a radius 454 889 fr) which is twice and 1.6 times the thickness of the material respectively.

TABELL IV ä Exempel ' 2T 1,6T 49-* zr'4o Trans" inga sprickor inga sprickor 50-* " "v Trans- inga sprickor inga sprickor 51- " 'H Trans. lätt apelsinyta lätt apelsinyta 52. " “, Trans. lätt apelsinyta lätt apeljinyta 53.* " “, Long. inga sprickor inga sprickor S4 . * " “, Long. inga sprickor inga sprickor 55, I' " ", Long. _ inga sprickor inga sprickor 55, H ", Long, lätt apelsínyta lätt apelsinyta É7. _" “, Long. lätt apelsinyta ' lätt apelsinyta * Glöagaa i kväve via 7oo°c (13oo°r) unaer 3 minuter Trans. = transversell provning Long. = longitudinell provning I ett försök att bestämma djupet och mängden av syre- och kväveupp- tagning från glödgningsprocessen utfördes en Anger-analys på Zirca- loy-4, vars resultat redovisas i tabell V.TABLE IV ä Example '2T 1,6T 49- * zr'4o Trans "no cracks no cracks 50- *" "v Trans- no cracks no cracks 51-"' H Trans. light orange surface light orange surface 52. "", Trans. light orange surface light orange surface 53. * "“, Long. no cracks no cracks S4. * "", Long. No cracks no cracks 55, I '"", Long. _ No cracks no cracks 55, H ", Long, light orange surface light orange surface É7. _ "“, Long. Light orange surface 'light orange surface * Glöagaa in nitrogen via 7oo ° c (13oo ° r) unaer 3 minutes Trans. = Transverse test Long. = Longitudinal test In an attempt to determine the depth and amount of oxygen and nitrogen uptake - removal from the annealing process, an Anger analysis was performed on Zircaloy-4, the results of which are reported in Table V.

'Cu fil 454 889 Avwuflmvmfiflflvmwflmwvd HV vwmmvvos Bowww u m4 æ.H ll w.æß em. m.H ll om. m.Hfl m.m wooß m.N Il w.mm mn. m.H ll cv. ßw.fi m.hfi M4 >H wa. || ß.fim Nm. vw. Il ll w.N m.m Moooß mw. l| fi.mh Nm. mm. || Hm. w.Nfi m.m moofi m.N Ii m.oß hv. mm. FN. nn. v.mH ß.æ md HHH No. ll m.øa mm. nu. ll ll æm. m.a Awoomv mmm ll ll N.Næ bh. ll II mu.m N.N ø.aH äoofi N.m II m.flß ll A.fi Nu. h.fl m.NH ~.m M4 HH mm. li w.mm mm. ma. |l Il mm. vm.A Awocwv mmm ll A.~ o.mm || mm. Nß. mm. ø.m fl.NN M4 H am m uu cm mm w 2 O U owmfl Hmmfimxm > flAHm 454 889 Exempel I representerar oglödgat material i utgångstillståndet.'Cu fi l 454 889 Avwu fl mvm fiflfl vmw fl mwvd HV vwmmvvos Bowww u m4 æ.H ll w.æß em. m.H ll om. m.H fl m.m wooß m.N Il w.mm mn. m.H ll cv. ßw. fi m.h fi M4> H wa. || ß. fi m Nm. vw. Il ll w.N m.m Moooß mw. l | m .mh Nm. mm. || Hm. w.N fi m.m moo fi m.N Ii m.oß hv. mm. U.N. nn. v.mH ß.æ md HHH No. ll m.øa mm. now. ll ll æm. m.a Awoomv mmm ll ll N.Næ bh. ll II mu.m N.N ø.aH äoo fi N.m II m. fl ß ll A. fi Nu. h. fl m.NH ~ .m M4 HH mm. li w.mm mm. ma. | l Il mm. vm.A Awocwv mmm ll A. ~ o.mm || mm. Nß. mm. ø.m fl. NN M4 H am m uu cm mm w 2 O U owm fl Hmm fi mxm> fl AHm 454 889 Example I represents unannealed material in the initial state.

Exempel II glödgades under 10 minuter vid 675°C (1250°F) i rent kväve. Exemplen III och IV glödgades under 5 minuter vid 67500 (1250°F) i kväve. Emellertid upptäcktes det att ugnen läckte under dessa exempel, och därför en väsentlig kvantitet luft befann sig i ugnen under glödgningen. Även.om det mesta av den ovan beskrivna glödgningen i kväve utför- des vid 700°C (1300°F) under 5 minuter kan glödgningen i kväve ge- nomföras vid lägre och högre temperatur inverterat proportionellt mot uppehållstiden av materialet i ugnen. Därför är det möjligt att tillverka en acceptabel produkt vid temperaturer från 5250 till 87500 (1000° till 1600°F) och behandlingetider från å minut till 15 minu- ter. Parametrarna kan sålunda variera från 1 minut vid 67500 (1250°F) :in 5 minuten vid'65o°c (1zoo°r) :in 15 minuter vid 6oo°c (11oo°F).Example II was annealed for 10 minutes at 675 ° C (1250 ° F) in pure nitrogen. Examples III and IV were annealed for 5 minutes at 67500 (1250 ° F) in nitrogen. However, it was discovered that the furnace was leaking during these examples, and therefore a significant quantity of air was in the furnace during annealing. Although most of the nitrogen annealing described above was performed at 700 ° C (1300 ° F) for 5 minutes, the nitrogen annealing can be performed at lower and higher temperatures inverted in proportion to the residence time of the material in the furnace. Therefore, it is possible to manufacture an acceptable product at temperatures from 5250 to 87500 (1000 ° to 1600 ° F) and treatment times from å minute to 15 minutes. Thus, the parameters can vary from 1 minute at 670000 (1250 ° F): in 5 minutes at 65 ° C (1000 ° F): in 15 minutes at 600 ° C (11 ° F).

Det viktiga är att temperaturen och tiden sammanfaller för en tid som är tillräcklig för att orsaka en fullständig omkristallisering men inte längre. Dei hem befunnite ett över e75°c ( 16oo°F) även under en kort tid, det uppstår diffusion av kväve in i materialet, som ger problem med missfärgning. Likeiedee vid tider under e minut blir behandlingen otillräcklig för att erhålla fullständig omkristalli- sering.The important thing is that the temperature and time coincide for a time that is sufficient to cause a complete recrystallization but no longer. Dei hem befunnite an above e75 ° c (16oo ° F) even for a short time, there is diffusion of nitrogen into the material, which causes problems with discoloration. Similarly, at times below one minute, the treatment becomes insufficient to obtain complete recrystallization.

Som sammanfattning av denna beskrivning framställer den föreliggande uppfinningen en ekonomisk metod för kontinuerlig glödgning av zirko- nium V och legeringar därav för erhållande av en överlägsen pro- dukt. Modifikationer är möjliga inom området för denna uppfinning.To summarize this description, the present invention provides an economical method for continuous annealing of zirconium V and alloys thereof to obtain a superior product. Modifications are possible within the scope of this invention.

-Iw-Iw

Claims (2)

454 889 Patentkrav454,889 Patent claims 1. Förfarande för att kontinuerligt glödga zirkoniummetall øch legeringar därav, k ä n n e t e c k n a t därav, att zirkoniummetallen eller -legeringen kontinuerligt bringas att passera genom en glödgningsugn innehållande en atmosfär av kväve under upprätthållande av metallen vid en temperatur mellan 525 och 875°C under en temgg- raturberøende tid av mellan 0,5 och 15 minuter.A process for continuously annealing zirconium metal and alloys thereof, characterized in that the zirconium metal or alloy is continuously passed through an annealing furnace containing an atmosphere of nitrogen while maintaining the metal at a temperature between 525 and 875 ° C for one hour. ratur dependent time of between 0.5 and 15 minutes. 2. Förfarande enligt krav 1, k ä n n e t e c k n a t av, att metallen har formen av ett band av zirkonium- legering.2. A method according to claim 1, characterized in that the metal is in the form of a band of zirconium alloy.
SE8105889A 1980-11-03 1981-10-06 PROCEDURE FOR CONTINUOUS GLODGA ZIRCONIUM SE454889B (en)

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US20369780A 1980-11-03 1980-11-03

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SE454889B true SE454889B (en) 1988-06-06

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JP (1) JPS5798662A (en)
DE (1) DE3143566C2 (en)
FR (1) FR2493347A1 (en)
GB (1) GB2086945B (en)
SE (1) SE454889B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3428954A1 (en) * 1984-08-06 1986-02-13 Kraftwerk Union AG, 4330 Mülheim SHELL TUBE MADE OF A ZIRCONIUM ALLOY, IN PARTICULAR FOR A CORE REACTOR FUEL AND METHOD FOR PRODUCING THIS SHELL TUBE
FR2575764B1 (en) * 1985-01-10 1992-04-30 Cezus Co Europ Zirconium PROCESS FOR MANUFACTURING A STRIP OF ZIRCONIUM ALLOY ZIRCALOY 2 OR ZIRCALOY 4 RESTORED, AND STRIP OBTAINED
US4717428A (en) * 1985-08-02 1988-01-05 Westinghouse Electric Corp. Annealing of zirconium based articles by induction heating
US4671826A (en) * 1985-08-02 1987-06-09 Westinghouse Electric Corp. Method of processing tubing
US5188676A (en) * 1991-08-23 1993-02-23 General Electric Company Method for annealing zircaloy to improve nodular corrosion resistance
DE10111109A1 (en) * 2001-03-08 2002-10-31 Deutsche Titan Gmbh Process for producing a titanium foil with a nitrided surface coating

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR399977A (en) * 1908-05-11 1909-07-13 Edouard Marc Daniel Hirsch Process for annealing metals
FR1530150A (en) * 1967-07-03 1968-06-21 Messer Griesheim Gmbh Shielding gas for metallurgical needs
JPS5837383B2 (en) * 1980-02-18 1983-08-16 住友金属工業株式会社 Continuous annealing method for titanium and titanium alloy strips

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DE3143566A1 (en) 1982-09-02
SE8105889L (en) 1982-05-04
FR2493347B1 (en) 1984-12-28
DE3143566C2 (en) 1985-11-07
JPH0154427B2 (en) 1989-11-17
FR2493347A1 (en) 1982-05-07
JPS5798662A (en) 1982-06-18
GB2086945A (en) 1982-05-19
GB2086945B (en) 1984-03-21

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