[go: up one dir, main page]

US3573998A - Method of heat-treating tungsten-base alloys - Google Patents

Method of heat-treating tungsten-base alloys Download PDF

Info

Publication number
US3573998A
US3573998A US636835A US3573998DA US3573998A US 3573998 A US3573998 A US 3573998A US 636835 A US636835 A US 636835A US 3573998D A US3573998D A US 3573998DA US 3573998 A US3573998 A US 3573998A
Authority
US
United States
Prior art keywords
carbon
tungsten
heat
alloy
temperature
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
Application number
US636835A
Inventor
Robert Walter Broomfield
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Imperial Metal Industries Kynoch Ltd
Original Assignee
Imperial Metal Industries Kynoch Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Imperial Metal Industries Kynoch Ltd filed Critical Imperial Metal Industries Kynoch Ltd
Application granted granted Critical
Publication of US3573998A publication Critical patent/US3573998A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S72/00Metal deforming
    • Y10S72/70Deforming specified alloys or uncommon metal or bimetallic work

Definitions

  • Tungsten-base alloys have been used in applications involving the very high melting point of tungsten.
  • Ductility is improved by breaking down the cast structure of tungsten and extrusion has hitherto been the only reliable method of so doing.
  • the products of extrusion are, however, long thin bars which are unsuitable for rolling to sheet or for shape-forging.
  • 'Forging is the most suitable primary working process for producing sheet-bar for rolling and for producing more complex shapes, such as, for example, rocket nozzles.
  • pure tungsten cannot be forged satisfactorily below 1700 C., but the addition of small amounts of carbon improves the forgeability of tungsten, so much so, that forging can be carried out at much lower temperatures.
  • 0.03 wt. percent carbon tungsten can be forged at 900 C.
  • a method of heattreating an alloy of tungsten containing 0.006-0.07% carbon comprises heating the alloy to a temperature of l700l900 C. for at least 10 minutes and cooling to 900 C. at a constant rate over a period of at least 1 hour, said treatment being carried out in a non-oxidising environment.
  • a useful commercial range of composition includes a carbon content of 0.01-0.05
  • the binary tungsten carbon alloy may be further strengthened at high operating temperatures by the addition of one or more alloying constituents, up to 10% in total, as follows: up to 10% molybdenum, up to 2% tantalum, up to 1% niobium or up to 0.5% zirconium. These elements strengthen the alloy at very high temperatures and ternary alloys may be used in preference to the binary alloy where conditions of service are particularly arduous, for example, in rocket nozzles where the hottest propellants are used.
  • Treatment is preferably carried out in a vacuum and this includes heating and cooling. At the temperature of treatment oxidation is very rapid and oxygen must be excluded. Slight oxidation, however, is tolerable.
  • the preferred solution treatment is 30 minutes at 1800 C. and the preferred cooling rate is 8 C. minute. Below 900 C. the cooling rate is unimportant, as carbon does not readily diffuse below that temperature.
  • the improvement in forgeabilty brought about by the treatment is believed to be due to the presence of a dispersion of carbides of a particle size conducive to a favourable dislocation pattern.
  • Relatively large particles of W C (1-2 microns) which have many dislocations associated with them, possibly produced by differences in thermal contraction between tungsten and W C are belived to be responsible for improved forgeability.
  • Small particles less than 0.1 micron in size often form on dislocations, and are likely to hinder their movement and thereby increase the resistance to deformation.
  • the elfect of the heat-treatment in accordance with the invention is believed to eliminate the line particles by taking them into solution and reprecipitating the carbon on the large particles. Then the dislocations are no longer pinned, and can move more freely.
  • an alloy containing 0.02% carbon would crack on forging at 600 C. whether heat-treated or as-cast. If heat-treated, this alloy would forge .without cracking at 800 C., but if it were as-cast it would crack at 800 C. Even in the as-cast condition this alloy would forge satisfactorily at 1200 C.
  • the lower curve has an almost linear portion extending from about 0.005-0.04% carbon which has a minimum forging temperature of about 700 C. Beyond 0.04% the curve rises and whilst the exact path is not shown, there is reason to believe that the limit of forgeability at 0.07% carbon is about 1100 C. At low carbon contents, the curve rises very steeply and below 0.005% carbon, the alloy rapidly becomes forgeable only at very high temperatures.
  • the range of carbon content over which the alloys treated in accordance with the invention may be forged at temperatures below 1100 C. is about 0.006-0.07% which extends the previously known range of 0.015-0.04% without heattreatment by a factor of about 2.6. Variations in carbon content are thus less serious.
  • Carbon contents above 0.04% are not required in high temperature applications such as rocket nozzles as the effect of increased carbon content is to decrease the. melting point.
  • the heat-treatment of the invention enables alloys of very low carbon content, and hence very high melting point, to be forged at about 800 C.
  • the heating-treatment makes it possible to produce articles in a tungsten-base alloy containing 0.0060.0 7% of carbon, such as rocket nozzles, by heating a cast ingot to 1700-1900 C., cooling to 900 C. at a constant rate over a period of at least one hour, forging to the required shape at a temperature in the region of 1100" C.
  • the alloy contains one or more of the following alloying constituents up to 10% in total: 010% molybdenum, 02% tantalum, 0l% niobium, 00.5% zirconium.
  • a method of producing a rocket nozzle from a cast ingot of a tungsten-base alloy containing about 0.005 to about 0.04% carbon comprising heating the cast ingot to a temperature of l7001900 C. for at least 10 minutes, and cooling to 900 C. at a constant rate over a period of at least one hour in a vacuum, and forging to the required shape.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Forging (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A METHOD OF HEAT-TREATING TUNGSTEN-BASE ALLOYS CONTAINING ABOUT 0.005 TO ABOUT 0.0490 CARBON AND OPTIONALLY MOLYBDENUM, TANTALUM, NIOBIUM AND ZIRCONIUM TO RENDER THE ALLOY FORGEABLE BELOW 1100*C., IN WHICH THE ALLOY IS HEATED BETWEEN 1700 AND 1900*C. AND COOLED AT A CONSTANT RATE OVER A PERIOD OF ONE HOUR TO A TEMPERATURE OF 900*C.

Description

FORGING TEMPERATURE "c April 6. 1911 RQWYBRQQMEIELI': 3,573,998
IB'IBOD OF HEAT-TREATING TUNGSTBN-BASE ALLOYS Filed May 8, 1967 f CAST TER HEAT aoo T REATMENT NCERTNN |;5oo\
LOOQ o -02 -04 -06 08 -lo CARBON CONTENT WEI,
MQ/ M Patented Apr. 6, 1971 3,573,998 METHOD OF HEAT-TREATING TUNGSTEN-BASE ALLOYS Robert Walter Broomfield, Sutton Coldfield, England,
assignor to Imperial Metal Industries (Kynoch) Limited, Birmingham, England Filed May 8, 1967, Ser. No. 636,835 Claims priority, applicafion Great Britain, May 17, 1966, 21,818/ 66 Int. Cl. C21d 1/00; C2215 1/18 US. Cl. 148-115 Claims ABSTRACT OF THE DISCLOSURE BACKGROUND OF THE INVENTION (1) Field of the invention This invention relates to a method of heat-treating tungsten base alloys containing carbon and is particularly applicable to cast material.
(2) Description of prior art Tungsten-base alloys have been used in applications involving the very high melting point of tungsten. Components made of this metal, for example rocket nozzles, have hitherto been fabricated by methods which are not very satisfactory. Machining of nozzles directly from cast material is a =difficult and wasteful method. Furthermore, cast tungsten is very brittle and diflicult to work.
Ductility is improved by breaking down the cast structure of tungsten and extrusion has hitherto been the only reliable method of so doing. The products of extrusion are, however, long thin bars which are unsuitable for rolling to sheet or for shape-forging.
'Forging is the most suitable primary working process for producing sheet-bar for rolling and for producing more complex shapes, such as, for example, rocket nozzles. As-cast, pure tungsten cannot be forged satisfactorily below 1700 C., but the addition of small amounts of carbon improves the forgeability of tungsten, so much so, that forging can be carried out at much lower temperatures. At the optimum composition, 0.03 wt. percent carbon, tungsten can be forged at 900 C.
Although this is a notable improvement, there are two drawbacks associated with it:
(a) The addition of 0.03% carbon to tungsten lowers the melting point from 3400 C. to about 2800 C. Thus for very high temperature applications such as in rockets using the hottest propellants, melting may occur.
(b) The range of carbon content over which alloys are forgeable at the typical forging temperature (1100 C.) is rather narrow 0.0l5-0.04%. Because of the variability of carbon losses during melting, it may not be possible to maintain the composition of ingots on a production basis within this narrow range, and consequently the forgeability may be adversely affected.
SUMMARY OF THE INVENTION We have found that the forgeability of tungsten carbon alloys may be improved by heat-treatment.
According to the present invention, a method of heattreating an alloy of tungsten containing 0.006-0.07% carbon comprises heating the alloy to a temperature of l700l900 C. for at least 10 minutes and cooling to 900 C. at a constant rate over a period of at least 1 hour, said treatment being carried out in a non-oxidising environment.
A useful commercial range of composition includes a carbon content of 0.01-0.05 The binary tungsten carbon alloy may be further strengthened at high operating temperatures by the addition of one or more alloying constituents, up to 10% in total, as follows: up to 10% molybdenum, up to 2% tantalum, up to 1% niobium or up to 0.5% zirconium. These elements strengthen the alloy at very high temperatures and ternary alloys may be used in preference to the binary alloy where conditions of service are particularly arduous, for example, in rocket nozzles where the hottest propellants are used.
Treatment is preferably carried out in a vacuum and this includes heating and cooling. At the temperature of treatment oxidation is very rapid and oxygen must be excluded. Slight oxidation, however, is tolerable.
The preferred solution treatment is 30 minutes at 1800 C. and the preferred cooling rate is 8 C. minute. Below 900 C. the cooling rate is unimportant, as carbon does not readily diffuse below that temperature.
The success of the treatment depends largely upon the rate of cooling since, as will be described later, it is believed that the particle size of carbides plays an important part in the forgeability of the alloy. If the cooling rate is too high, a large number of fine particles is precipitated and this is undesirable, whilst a very slow rate of cooling is uneconomic. We have found that a period of about :1 hour is the highest rate of cooling which will produce the desired improvement.
The improvement in forgeabilty brought about by the treatment is believed to be due to the presence of a dispersion of carbides of a particle size conducive to a favourable dislocation pattern. Relatively large particles of W C (1-2 microns) which have many dislocations associated with them, possibly produced by differences in thermal contraction between tungsten and W C are belived to be responsible for improved forgeability. Small particles less than 0.1 micron in size often form on dislocations, and are likely to hinder their movement and thereby increase the resistance to deformation.
The elfect of the heat-treatment in accordance with the invention is believed to eliminate the line particles by taking them into solution and reprecipitating the carbon on the large particles. Then the dislocations are no longer pinned, and can move more freely.
DESCRIPTION OF DRAWING The invention is further illustrated by reference to the accompanying drawing which is a graph showing curves corresponding to forgeability at various temperatures and carbon contents.
The influence of the heat-treatment on the forgeability of tungsten-carbon alloys is shown in the drawing in which the curves mark the lower limits of temperature relative to carbon content at which sound forgings can be made. The upper curve shows the forgeability of as-ca'st alloys and the lower curve that of alloys heat-treated in accordance with the invention. Alloys forged at temperatures above the appropriate curve are sound and those forged below are cracked.
As can be seen from the drawing, an alloy containing 0.02% carbon would crack on forging at 600 C. whether heat-treated or as-cast. If heat-treated, this alloy would forge .without cracking at 800 C., but if it were as-cast it would crack at 800 C. Even in the as-cast condition this alloy would forge satisfactorily at 1200 C.
It will be seen that the lower curve has an almost linear portion extending from about 0.005-0.04% carbon which has a minimum forging temperature of about 700 C. Beyond 0.04% the curve rises and whilst the exact path is not shown, there is reason to believe that the limit of forgeability at 0.07% carbon is about 1100 C. At low carbon contents, the curve rises very steeply and below 0.005% carbon, the alloy rapidly becomes forgeable only at very high temperatures. The range of carbon content over which the alloys treated in accordance with the invention may be forged at temperatures below 1100 C. is about 0.006-0.07% which extends the previously known range of 0.015-0.04% without heattreatment by a factor of about 2.6. Variations in carbon content are thus less serious.
Carbon contents above 0.04% are not required in high temperature applications such as rocket nozzles as the effect of increased carbon content is to decrease the. melting point. The heat-treatment of the invention enables alloys of very low carbon content, and hence very high melting point, to be forged at about 800 C.
The heating-treatment makes it possible to produce articles in a tungsten-base alloy containing 0.0060.0 7% of carbon, such as rocket nozzles, by heating a cast ingot to 1700-1900 C., cooling to 900 C. at a constant rate over a period of at least one hour, forging to the required shape at a temperature in the region of 1100" C.
I claim:
1. A method of improving the forgeability of a tungsten-base alloy containing about 0.005 to about 0.04% carbon to render said alloy forgeable at a minimum temperature of about 700 C. Without cracking, com
prising heating the alloy to a temperature of 17001900 C. for at least 10 minutes and cooling to 900 C. at a constant rate over a period of at least one hour, said treatment being carried out in a non-oxidizing environment.
2. A method as claimed in claim 1 in which the alloy contains one or more of the following alloying constituents up to 10% in total: 010% molybdenum, 02% tantalum, 0l% niobium, 00.5% zirconium.
3. A method as claimed in claim 1 in which the alloy is cooled at a rate of 8 C. per minute.
4. A method as claimed in claim 1 in which the alloy is heated to a temperature of 1800" C.
5. A method of producing a rocket nozzle from a cast ingot of a tungsten-base alloy containing about 0.005 to about 0.04% carbon comprising heating the cast ingot to a temperature of l7001900 C. for at least 10 minutes, and cooling to 900 C. at a constant rate over a period of at least one hour in a vacuum, and forging to the required shape.
CHARLES N. LOVELL, Primary Examiner US. Cl. X.R. 72700; 148-133
US636835A 1966-05-17 1967-05-08 Method of heat-treating tungsten-base alloys Expired - Lifetime US3573998A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB21818/66A GB1167134A (en) 1966-05-17 1966-05-17 A Method of Heat-Treating Tungsten-Base Alloys.

Publications (1)

Publication Number Publication Date
US3573998A true US3573998A (en) 1971-04-06

Family

ID=10169333

Family Applications (1)

Application Number Title Priority Date Filing Date
US636835A Expired - Lifetime US3573998A (en) 1966-05-17 1967-05-08 Method of heat-treating tungsten-base alloys

Country Status (4)

Country Link
US (1) US3573998A (en)
AT (1) AT275172B (en)
DE (1) DE1558787B2 (en)
GB (1) GB1167134A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102517426A (en) * 2011-12-21 2012-06-27 贵州航天控制技术有限公司 Heat treatment method of high specific gravity alloy

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005021982B4 (en) * 2005-05-12 2007-04-05 Rheinmetall Waffe Munition Gmbh Process for the preparation of a penetrator

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE637945A (en) * 1963-09-13

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102517426A (en) * 2011-12-21 2012-06-27 贵州航天控制技术有限公司 Heat treatment method of high specific gravity alloy

Also Published As

Publication number Publication date
GB1167134A (en) 1969-10-15
AT275172B (en) 1969-10-10
DE1558787B2 (en) 1971-01-07
DE1558787A1 (en) 1971-01-07

Similar Documents

Publication Publication Date Title
US3686041A (en) Method of producing titanium alloys having an ultrafine grain size and product produced thereby
US2974076A (en) Mixed phase, alpha-beta titanium alloys and method for making same
US3489617A (en) Method for refining the beta grain size of alpha and alpha-beta titanium base alloys
US3481799A (en) Processing titanium and titanium alloy products
US3642543A (en) Thermomechanical strengthening of the superalloys
JPH07504711A (en) Alloy of molybdenum, rhenium and tungsten
US2968586A (en) Wrought titanium base alpha-beta alloys of high creep strength and processing thereof
CN112322987B (en) Ultrahigh-strength steel wire for electric arc additive manufacturing and preparation method
US3645800A (en) Method for producing wrought zirconium alloys
US2241815A (en) Method of treating copper alloy castings
JPWO2003091468A1 (en) Titanium alloy forging method and titanium alloy forging
US2829048A (en) High damping alloy and members prepared therefrom
US3573998A (en) Method of heat-treating tungsten-base alloys
US2281691A (en) Process for heat treating copper alloys
US2637672A (en) Process of producing bolts
JPS6132386B2 (en)
US3595645A (en) Heat treatable beta titanium base alloy and processing thereof
US2798827A (en) Method of casting and heat treating nickel base alloys
US3379520A (en) Tantalum-base alloys
US3230119A (en) Method of treating columbium-base alloy
US3243290A (en) Tantalum base alloy
US2666698A (en) Alloys of titanium containing aluminum and iron
US3021211A (en) High temperature nickel base alloys
US3390983A (en) Tantalum base alloys
US3366513A (en) Heat treatment of niobium alloys