US3333994A - Process for the manufacture of products of beryllium or beryllium alloy - Google Patents

Process for the manufacture of products of beryllium or beryllium alloy Download PDF

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US3333994A
US3333994A US401862A US40186264A US3333994A US 3333994 A US3333994 A US 3333994A US 401862 A US401862 A US 401862A US 40186264 A US40186264 A US 40186264A US 3333994 A US3333994 A US 3333994A
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beryllium
ingot
tubes
temperature
alloy
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US401862A
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Mallen Jose
Weisz Michel
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
    • G21C3/02—Fuel elements
    • G21C3/04—Constructional details
    • G21C3/06—Casings; Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/32—Lubrication of metal being extruded or of dies, or the like, e.g. physical state of lubricant, location where lubricant is applied
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C25/00—Alloys based on beryllium
    • 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
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
    • G21C3/02—Fuel elements
    • G21C3/04—Constructional details
    • G21C3/06—Casings; Jackets
    • G21C3/07—Casings; Jackets characterised by their material, e.g. alloys
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

Definitions

  • the present invention relates to improvements in processes for the manufacture of beryllium products which are intended notably for aviation, astronautics and atomic energy.
  • tubes of this type have proved incapable of meeting certain requirements in regard to casings for nuclear fuels.
  • the casing is at a temperature which is determined by its position, the neutron balance of the reactor, the speed of the cooling fluid, etc., and it is normally sufiiciently hot to afford relief from any stresses.
  • the entry temperature of the fluid usually 200-250 C., is of great importance.
  • Tubes obtained by powder metallurgy do not possess such ductility in a sufficient degree. Efforts have therefore been directed to the production of tubes possessing this essential form of ductility and it has been discovered that, to some extent, the longitudinal ductility and the grain size are only of secondary importance.
  • the present invention therefore has the object of providing a process for the preparation of products of beryllium or beryllium alloy and particularly tubes, which more fully satisfies than hitherto the various practical re- 3,333,994 Patented Aug. 1, 1967 quirements, and in particular permits of obtaining a less fragile product of more favourable texture which is not detrimentally affected by maintenance for long periods at temperatures of the order of 700 C., which is much cleaner from the viewpoint of inclusions, exhibits few intergranular flaws and above all possesses distinctly higher transverse ductility.
  • the invention resides mainly in that-while an ingot of cast beryllium or beryllium alloy, optionally subjected to a compression, is used as starting material-the said ingot is subjected, in the course of its shaping to at least one cold working operation, optionally followed by a tepid drawing, a straightening by stress relief with imparted deformation at a temperature close to that of the recrystallisation of the metal, and followed by a controlled recrystallisation annealing.
  • the invention further comprises, apart from this main feature, certain other features which are preferably used 'at the same time, and which are to be considered separately or in any technically possible combinations:
  • the said cold working operation or operations consist in impact extrusion, the metal being optionally coated with a thin layer of silver,
  • the said cold working operation or operations consist in extrusion under a casing, which casing may notably consist of soft steel,
  • the said cold working operation or operations consist in a pre-extrusion under a thin casing followed by an extrusion under a thick casing,
  • the extent of the extrusion is at least equal to 50.
  • cast metal as starting material, instead of sintered metal as usual, is one of the most important features of the present invention because it shows that cold-worked cast metal is substantially free from hot fragility, that its texture is more favourable than that of cold-worked sintered metal, that maintenance at 600- 700 C. for long periods is beneficial to the cold-worked cast metal, while it is harmful to cold-worked sintered metal, that inclusion radiographs have revealed higher cleanness of the cold-worked cast metal, and finally that, although its presentation and its surface appearance seem to be less good, it is less subject to defects such as intergranular microcraoks, which are harmful to transverse ductility in the case of tubes.
  • Extruded sintered sheet bar 50 400 Extruded cast sheet bar 250 extrusion or the conventional extrusion under a casing may be used, but the second method gives greater lengths of more uniform tubes, as will hereinafter be seen with reference to the following example.
  • the tubes of cold-worked cast metal according to the present invention may also be subjected to a tepid drawing which improves the tolerances of the surface condition, and gives greater pliability in the controllled recrystallisation treatments.
  • drawing passes of to at 450 C. are possible without intermediate annealing.
  • the tubes thus prepared are thereafter subjected to stress relief followed by annealing at a temperature close to the recrystallisation temperature, i.e. between 550 and 750 C., which process improves the elastic limit at elevated temperature and the ductility of the beryllium.
  • the bar thus obtained is cut into sections and pierced to supply the billets intended for the extrusion of tubes.
  • a second extrusion is thereafter performed at 950 C. at a speed of 27 mm./second and to a cold-working degree or an area reduction of 15.
  • the trueing of the tubes is thereafter effected by deformation imparted in tension, in the course of which a considerable stress relief occurs at 650 C. in half an hour, and annealed at 750 C. for 4 hours.
  • the product obtained is more ductile and less fragile than an equivalent product prepared from sintered metal, as is shown by comparison of the curves A and B of the single figure.
  • Curve A corresponds to a beryllium tube obtained by the process of the invention.
  • Curve B corresponds to a sintered tube.
  • Dr% is the percentage of elongation at the moment of rupture of a test bar subject to traction.
  • a method for manufacturing tubes of beryllium and beryllium allloy comprising the steps of first working a cast ingot of beryllium and beryllium alloy at about 950 C. with an area reduction of about 6, then further working said ingot at about 950 C. with an area of reduction of about 15, then subjecting the drawn ingot to stress relief with plastic deformation in tension at a temperature approaching recrystallization temperature of the metal in the range of 550750 C. and then annealing at a temperature of about 750 C. for about four hours.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Forging (AREA)
  • Powder Metallurgy (AREA)
  • Extrusion Of Metal (AREA)

Description

Aug. 1, 1967 .MALLEN ET AL 3,333,994 3 PROCESS FOR THE MANUFACTURE OF PRODUCTS OF BERYLLIUM' OR BERYLLIUM ALLOY Filed Oct. '6, 1964- 0,2 impel-afar:
United States Patent 3,333,994 PROCESS FOR THE MANUFACTURE OF PRODUCTS OF BERYLLIUM OR BERYL- LIUM ALLOY Jos Mallen, Paris and Michel Weisz, Orsay, France, as-
signors to Commissariat a IEnergie Atomique, Paris, France Filed Oct. 6, 1964, Ser. No. 401,862 Claims priority, application France, Oct. 25, 1963, 951,895 7 Claims. (Cl. 14811.5)
The present invention relates to improvements in processes for the manufacture of beryllium products which are intended notably for aviation, astronautics and atomic energy.
It concerns more particularly processes of this type which are concerned with the production of beryllium tubes, and more particularly tubes suitable for the casing of fuel elements of nuclear reactors.
Since the beginning of the utilisation of beryllium in aircraft and then in space craft, and finally as a nuclear material, for which fields it is particularly suitable by virtue of its remarkable physical properties, the desired beryllium products have always been made from billets or blooms of sintered beryllium. Onlysome parts of simple shape, such as sheets, have been obtainable from cast metal, and even then it has been necessary to effect a grain refinement in order that this material may have acceptable mechanical characteristics.
Endeavours have therefore been made to improve the ductility of beryllium tubes and for this reason recourse has hitherto been had to powder metallurgy for the production of such tubes, since the sintered metal has a much finer grain than the cast metal, as also much higher longitudinal ductility (in the direction of the cold working at low temperature).
However, despite many efforts to increase the threedimensional ductility, tubes of this type have proved incapable of meeting certain requirements in regard to casings for nuclear fuels.
Of the many stresses which are set up in the course of the operation of the reactor, the casing of a fuel pencil, i.e. of a rod of very small diameter in relation to its length, must notably withstand with an appropriate safety margin those which correspond to the thermal stresses resulting from its association with the fuel (each of these members has its own programme temperature and its own coefficient of expansion).
During continuous operation, the casing is at a temperature which is determined by its position, the neutron balance of the reactor, the speed of the cooling fluid, etc., and it is normally sufiiciently hot to afford relief from any stresses.
In transient operation, particularly during cooling, the situation is more critical owing to the thermal stresses set up in the casing. In this respect, the entry temperature of the fluid, usually 200-250 C., is of great importance.
It has been found that with a casing, the major problem is to obtain sufiicient transverse ductility at low temperature in order to avoid rupture.
Tubes obtained by powder metallurgy do not possess such ductility in a sufficient degree. Efforts have therefore been directed to the production of tubes possessing this essential form of ductility and it has been discovered that, to some extent, the longitudinal ductility and the grain size are only of secondary importance.
The present invention therefore has the object of providing a process for the preparation of products of beryllium or beryllium alloy and particularly tubes, which more fully satisfies than hitherto the various practical re- 3,333,994 Patented Aug. 1, 1967 quirements, and in particular permits of obtaining a less fragile product of more favourable texture which is not detrimentally affected by maintenance for long periods at temperatures of the order of 700 C., which is much cleaner from the viewpoint of inclusions, exhibits few intergranular flaws and above all possesses distinctly higher transverse ductility.
The invention resides mainly in that-while an ingot of cast beryllium or beryllium alloy, optionally subjected to a compression, is used as starting material-the said ingot is subjected, in the course of its shaping to at least one cold working operation, optionally followed by a tepid drawing, a straightening by stress relief with imparted deformation at a temperature close to that of the recrystallisation of the metal, and followed by a controlled recrystallisation annealing.
The invention further comprises, apart from this main feature, certain other features which are preferably used 'at the same time, and which are to be considered separately or in any technically possible combinations:
The said cold working operation or operations consist in impact extrusion, the metal being optionally coated with a thin layer of silver,
The said cold working operation or operations consist in extrusion under a casing, which casing may notably consist of soft steel,
The said cold working operation or operations consist in a pre-extrusion under a thin casing followed by an extrusion under a thick casing,
The extent of the extrusion is at least equal to 50.
In any case, the invention will be more readily understood from the following further description and the following example, which are, of course, given only by way of example. In the course of this description, reference will be made to the single figure which gives, as a function of temperature, the transverse ductility of the beryllium treated by the process according to the invention 'and of sintered beryllium.
The use of cast metal as starting material, instead of sintered metal as usual, is one of the most important features of the present invention because it shows that cold-worked cast metal is substantially free from hot fragility, that its texture is more favourable than that of cold-worked sintered metal, that maintenance at 600- 700 C. for long periods is beneficial to the cold-worked cast metal, while it is harmful to cold-worked sintered metal, that inclusion radiographs have revealed higher cleanness of the cold-worked cast metal, and finally that, although its presentation and its surface appearance seem to be less good, it is less subject to defects such as intergranular microcraoks, which are harmful to transverse ductility in the case of tubes.
The following table shows a comparison of the longitudinal and transverse ductilities of sintered and cast beryllium ingots:
Minimum temperature for an elongation of 10% Longitudinal Transverse (DL), 0. (Dr), Q o.
Extruded sintered sheet bar 50 400 Extruded cast sheet bar 250 extrusion or the conventional extrusion under a casing may be used, but the second method gives greater lengths of more uniform tubes, as will hereinafter be seen with reference to the following example.
The tubes of cold-worked cast metal according to the present invention may also be subjected to a tepid drawing which improves the tolerances of the surface condition, and gives greater pliability in the controllled recrystallisation treatments. Thus, drawing passes of to at 450 C. are possible without intermediate annealing.
The tubes thus prepared are thereafter subjected to stress relief followed by annealing at a temperature close to the recrystallisation temperature, i.e. between 550 and 750 C., which process improves the elastic limit at elevated temperature and the ductility of the beryllium.
There will therefore be given in the following an example of the production of beryllium tubes by the process according to the present invention.
There is used as starting material a cast beryllium ingot which is compressed for 2 minutes at 650 C. under a pressure of 10,000 bars, this compression having the object of eliminating any remaining small pipes and thus providing a clean ingot.
In the course of a pro-extrusion at 950 C., a billet in the form of a thin soft steel casing 2 mm. thick is coldworked to a degree or an area reduction of 6.
The bar thus obtained is cut into sections and pierced to supply the billets intended for the extrusion of tubes.
A second extrusion is thereafter performed at 950 C. at a speed of 27 mm./second and to a cold-working degree or an area reduction of 15.
The trueing of the tubes is thereafter effected by deformation imparted in tension, in the course of which a considerable stress relief occurs at 650 C. in half an hour, and annealed at 750 C. for 4 hours. As stated in the foregoing, the product obtained is more ductile and less fragile than an equivalent product prepared from sintered metal, as is shown by comparison of the curves A and B of the single figure.
Curve A corresponds to a beryllium tube obtained by the process of the invention. Curve B corresponds to a sintered tube. Dr% is the percentage of elongation at the moment of rupture of a test bar subject to traction.
Of course, the invention is in no way limited to the mode of application just referred to, or to the embodiment described, but covers all variants thereof, and notably the manufacture of all beryllium products from cast metal,
not only for nuclear uses, but also for requirements of aviation and astronautics.
What is claimed is:
1. A method for manufacturing tubes of beryllium and beryllium allloy comprising the steps of first working a cast ingot of beryllium and beryllium alloy at about 950 C. with an area reduction of about 6, then further working said ingot at about 950 C. with an area of reduction of about 15, then subjecting the drawn ingot to stress relief with plastic deformation in tension at a temperature approaching recrystallization temperature of the metal in the range of 550750 C. and then annealing at a temperature of about 750 C. for about four hours.
2. A method as described in claim 1, including the step of first compressing the cast ingot of berylflium and berryllium alloy at about 650 C.
3. A method as described in claim 1, including the step, after the further working step, of then tepid drawing said ingot at about 450 C.
4. A method as described in claim 1, said working steps comprising impact extrusion, the ingot being coated with a thin layer of silver.
5. A method as described in claim 1, said working steps consisting of extrusion under a casing of soft steel.
6. A method as described in claim 1, said first working step consisting of extrusion under a thin casing followed by said further working step of extrusion step under a thick casing.
7. A method as described in claim 1, said working steps consisting of hot extrusion of the ingot with an area reduction at least equal to :1.
References Cited UNITED STATES PATENTS 2,872,363 '2/1959 Macherey 14811.5 3,065,117 11/1962 Brown et al. 14813 3,234,052 2/1966 Wikle 148l1.5
FOREIGN PATENTS 868,064 5/1961 Great Britain.
884,108 12/1961 Great Britain.
884,410 12/1961 Great Britain.
919,423 2/1963 Great Britain.
DAVID L. RECK, Primary Examiner.
H. F. SAITO, Assistant Examiner.

Claims (1)

1. A METHOD FOR MANUFACTURING TUBES OF BERYLLIUM AND BERYLLIUM ALLOY COMPRISIG THE STEPS OF FIRST WORKING A CAST INGOT OF BERYLLIUM AND BERYLLIUM ALLOY AT ABOUT 950*C. WITH AN AREA REDUCTION OF ABOUT 6, THEN FURTHER WORKING SAID INGOT AT ABOUT 950*C. WITH AN AREA OF REDUCTION OF ABOUT 15, THEN SUBJECTING THE DRAWN INGOT TO STRESS RELIEF WITH PLASTIC DEFORMATION IN TENSION AT A TEMPERATURE APPROACHING RECRYSTALLIZATION TEMPERATURE OF THE METAL IN THE RANGE OF 550-750*C. AND THEN ANNEALING AT A TEMPERATURE OF ABOUT 750*C. FOR ABOUT FOUR HOURS.
US401862A 1963-10-25 1964-10-06 Process for the manufacture of products of beryllium or beryllium alloy Expired - Lifetime US3333994A (en)

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FR951895A FR1381453A (en) 1963-10-25 1963-10-25 Improvements in manufacturing processes for beryllium or beryllium alloy products

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BE (1) BE654077A (en)
CH (1) CH433778A (en)
DE (1) DE1290726B (en)
ES (1) ES305279A1 (en)
FR (1) FR1381453A (en)
GB (1) GB1085804A (en)
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LU (1) LU47164A1 (en)
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3483047A (en) * 1967-06-21 1969-12-09 Us Air Force Ductile polycrystalline beryllium
US3791878A (en) * 1971-03-25 1974-02-12 Kawecki Berylco Ind Method of obtaining ductile beryllium
US4017333A (en) * 1975-08-25 1977-04-12 Lockheed Missiles & Space Company, Inc. Fine grain beryllium bodies

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2872363A (en) * 1948-07-14 1959-02-03 Robert E Macherey Method of working beryllium
GB868064A (en) * 1958-02-13 1961-05-17 Atomic Energy Authority Uk Extrusion and drawing of beryllium
GB884108A (en) * 1959-10-06 1961-12-06 Atomic Energy Authority Uk Improvements in or relating to the fabrication of beryllium
GB884410A (en) * 1959-06-02 1961-12-13 Ti Group Services Ltd Manufacture of beryllium tubes
US3065117A (en) * 1959-08-19 1962-11-20 Babcock & Wilcox Co Process for the production of beryllium having increased ductility at high temperatures
GB919423A (en) * 1960-10-04 1963-02-27 Atomic Energy Authority Uk Metallurgical process for working beryllium
US3234052A (en) * 1961-07-28 1966-02-08 Brush Beryllium Co Beryllium sheet and method of producing same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2872363A (en) * 1948-07-14 1959-02-03 Robert E Macherey Method of working beryllium
GB868064A (en) * 1958-02-13 1961-05-17 Atomic Energy Authority Uk Extrusion and drawing of beryllium
GB884410A (en) * 1959-06-02 1961-12-13 Ti Group Services Ltd Manufacture of beryllium tubes
US3065117A (en) * 1959-08-19 1962-11-20 Babcock & Wilcox Co Process for the production of beryllium having increased ductility at high temperatures
GB884108A (en) * 1959-10-06 1961-12-06 Atomic Energy Authority Uk Improvements in or relating to the fabrication of beryllium
GB919423A (en) * 1960-10-04 1963-02-27 Atomic Energy Authority Uk Metallurgical process for working beryllium
US3234052A (en) * 1961-07-28 1966-02-08 Brush Beryllium Co Beryllium sheet and method of producing same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3483047A (en) * 1967-06-21 1969-12-09 Us Air Force Ductile polycrystalline beryllium
US3791878A (en) * 1971-03-25 1974-02-12 Kawecki Berylco Ind Method of obtaining ductile beryllium
US4017333A (en) * 1975-08-25 1977-04-12 Lockheed Missiles & Space Company, Inc. Fine grain beryllium bodies

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CH433778A (en) 1967-04-15
GB1085804A (en) 1967-10-04
BE654077A (en) 1965-02-01
IL22204A (en) 1968-03-28
FR1381453A (en) 1964-12-14
SE310947B (en) 1969-05-19
LU47164A1 (en) 1964-12-19
ES305279A1 (en) 1965-03-16
DE1290726B (en) 1969-03-13
NL6411480A (en) 1965-04-26

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