US3370945A - Magnesium-base alloy - Google Patents

Magnesium-base alloy Download PDF

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US3370945A
US3370945A US467771A US46777165A US3370945A US 3370945 A US3370945 A US 3370945A US 467771 A US467771 A US 467771A US 46777165 A US46777165 A US 46777165A US 3370945 A US3370945 A US 3370945A
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percent
alloy
magnesium
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calcium
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US467771A
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George S Foerster
John B Clark
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Dow Chemical Co
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Dow Chemical Co
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/02—Alloys based on magnesium with aluminium as the next major constituent

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  • Alloying constituent Weight percent Aluminum 0.l-l.75 Manganese 0.1-1.0 Calcium 0.05-0.6
  • the alloy of the invention exhibits excellent compressive yield strength and is weldable without stressrelief. Furthermore, the alloy exhibits good resistance to creep; it is readily workable and it is relatively inexpensive.
  • the binary magnesium base alloys containing aluminum are improved by the addition of manganese, i.e., they exhibit better strength properties and improved corrosion resistance. Now it has been found that the ternary magnesium base alloys containing certain proportions of aluminum and manganese are further improved by the addition of small amounts of calcium in the range of 0.05 to 0.6 percent by weight.
  • the calcium and aluminum contents of the alloy can be varied to obtain various combinations of desirable properties.
  • the alloy free from zinc additions exhibits desirable characteristics of Weldability, castability and rollability not found in the zinc containing alloy.
  • Commercially pure magnesium normally contains trace amounts of zinc. Incidental inclusion of zinc as an impurity from all sources should not exceed about 0.03 percent by weight of the total alloy.
  • high calcium in the range of about 0.3 percent by weight
  • low aluminum e.g., about 0.5 percent by weight
  • Aluminum to calcium ratios in such combinations are less than about 2.6.
  • the other type combination contains low calcium in the range of about 0.15 percent by weight and high aluminum, e.g., about 1.2 percent by weight.
  • This combination offers higher ductility, and better castability, weldability without stress-relief, and good workability.
  • Such alloy is most suitable where the alloy is to be cold worked whereby optimum strength is developed.
  • Aluminum to'calcium ratios in such combinations are greater than about 2.6 and the sum of the percent of aluminum 3,370,945 Patented F eb. 27, 1958 ICC plus the sum of the percent of calcium is less than about 2.2 percent.
  • the manganese content is in the range of 0.3 to about 0.8 percent.
  • the present alloy composition contains, by weight, from about 0.25 to abuot 1.5 percent of aluminum, from about 0.3 to about 0.8 percent of manganese, and from about 0.1 to about 0.4 percent of calcium, the balance being substantially commercially pure magnesium (purity about 99.8 percent).
  • Two especially preferred alloys have the following compositions, by Weight: 1) 0.5 percent of aluminum, 0.75 percent of manganese, 0.3 percent of calcium, and the balance magnesium, and (2) 1.25 percent of aluminuin', 0.50 percent of magnanese, 0.15 percent of calcium, and the balance magnesium.
  • the alloy may be made in the desired proportions according to the invention by melting together the alloy ingredients in proper proportions or by using hardeners of magnesium alloys containing the alloy constituents.
  • the manganese may be added by direct reduction of manganese halide added to the flux.
  • Protection from oxidation during alloying is effected by the use of a magnesium chloride-free saline flux as in conventional alloying.
  • the molten alloy may be flux refined by stirring the alloy with additional flux.
  • the sorefined alloy is allowed to settle and may then be separated from the flux as by decanting into a suitable casting mold, as for example, a slab mold for rolling stock or a billet mold for extrusion stock.
  • the flux-refined metal may be decanted into the holding pot of the die casting machine.
  • the present alloy exhibits better creep resistance than the frequently used commercial alloy having the ASTM designation AZ91B.
  • the molten alloy of the invention is normally cast into either rolling slabs or extrusion billets. Usually the external surface of the cast piece is removed, as by a scalping operation. Extrusion billets are preheated to about 600-900 F. and are then die-expressed from a heated container. Rolling slabs are heated to about 700950 F. and reduced in thickness to about 0.1 inch sheet by multiple passes through the rolls of a mill, reheating the metal as necessary to avoid cracking.
  • the so-rolled metal sheet is then finished in a number of Ways as desired.
  • the rolled metal may be annealed one hour at a temperature in the range of 700 to 950 F., quenched, and reduced by cold rolling at l to 2 percent per pass through steam heated rolls under conditions close to the cracking limit, and further annealedat a temperature in the range of 300 to 700 F.
  • This method is particularly applicable to the present alloy having a relatively high aluminum to calcium weight ratio.
  • the rolled metal may also be finished by heating about one hour at 700 to 950 F., warm rolling the sheet to final thickness in one pass through the rolls of the mill, the metal exciting from the rolls at a temperature of 300 to 800 F., and quenching the exciting metal. If desired, the quenched metal may be aged or annealed at a temperature in the range of 300 to 800 F.
  • the alloy of the invention exhibiting a relatively low aluminum to calcium weight ratio is desirably and conveniently finished without further rolling upon solution heat treating the rolled metal at a temperature in the range of about 850 to 950 F., after which the metal is immediately quenched, and thereafter aged at a temperature of about 300 to 350 F.
  • tions according to the invention were prepared and cast into respective rolling slabs (e.g., 2" x 4" x 8"
  • Each slab was treated as follows: the faces of the slabs were scalped to remove surface impurities or inclusions, the slab was heated to 700950 F. and reduced in thickness to about 0.1 inch sheet by multiple passes through the ro1ls of a mill, reheating the metal as necessary to avoid cracking.
  • the rolled metal was then either annealed one hour at 950 F. and quenched, or, annealed for one hour at 700 F. Some of this metal was brought to a hard temper condition by cold rolling, at 1 to 2 percent per pass through steam heated rolls under conditions close to the cracking limit, and further annealing (one hour at 300 F).
  • compositions according to the invention were prepared and cast both as extrusion stock and rolling stock.
  • Extrusion stock was scalped and heated to a temperature in the range 600900 F. and extruded into inch x inch strip at 700 F. from a 3-inch container at a rate of from about to about 100 feet per minute.
  • the so-obtained strip was aged 24 hours at 350 F.
  • Rolling stock was scalped and heated to a temperature in the range 700-950 F., then hot rolled starting with an initial temperature of 850 F., being reduced in thickness, by multiple passes through the rolls of a mill, from 2 inch to 0.1 inch.
  • the so-obtained sheet was solution heat treated one hour at 950 F., water quenched and aged 24 hours at 320 F.
  • the alloy of the invention possesses the characteristic lightness of magnesium and the simultaneous combination of weldability without stress-relief, strength, workability, and low cost.
  • the magnesium base alloy consisting essentially of from 0.1 to 1.75 percent by Weight of aluminum, from 0.1 to 1.0 percent by weight of manganese, from 0.05 to 0.6 percent by weight of calcium, and the balance substantially magnesium [free from Zinc], the combined total amount or aluminum and calcium in the alloy not exceeding 2.2 percent by weight.
  • the magnesium base alloy as in claim 1, in which the Weight ratio of the aluminum content to the calcium content is less than about 2.6 percent.
  • the magnesium base alloy consisting essentially of from 0.25 to about 1.5 percent by weight of aluminum, from 0.3 to about 0.8 percent by weight of manganese, from 0.1 to about 0.4- percent by weight of calcium, and the balance being substantially magnesium [free from zinc].
  • the magnesium base alloy consisting essentially of 6.
  • the magnesium base alloy consisting essentially of 1.2 percent by weight of aluminum, from 0.3 to 0.8 percent by weight of manganese, about 0.15 percent by weight of calcium, and the balance substantially magnesium [free from zinc], the weight ratio of calcium to aluminum being greater than about 2.6 percent, and the alloy being characterized by weldability without stressrelief and by good cold workability.

Description

United States Patent 3,370,945 MAGNESIUM-BASE ALLOY George S. Foerster, Midland, and John B. Clark, Detroit, Mich., assignors to The Dow Chemical Company, Midland, Micln, a corporation of Delaware No Drawing. Filed June 28, 1965, Ser. No. 467,771 6 Claims. (Cl. 75168) ABSTRACT OF THE DISCLOSURE This invention relates to a magnesium base alloy free from zinc and containing aluminum, manganese and calcium and having primarily the following composition:
Alloying constituent: Weight percent Aluminum 0.l-l.75 Manganese 0.1-1.0 Calcium 0.05-0.6
Balance, commercially pure magnesium.
Commercially pure magnesium is the purity grade metal as produced in electrolytic cells.
The alloy of the invention exhibits excellent compressive yield strength and is weldable without stressrelief. Furthermore, the alloy exhibits good resistance to creep; it is readily workable and it is relatively inexpensive.
The binary magnesium base alloys containing aluminum are improved by the addition of manganese, i.e., they exhibit better strength properties and improved corrosion resistance. Now it has been found that the ternary magnesium base alloys containing certain proportions of aluminum and manganese are further improved by the addition of small amounts of calcium in the range of 0.05 to 0.6 percent by weight. The calcium and aluminum contents of the alloy can be varied to obtain various combinations of desirable properties. The alloy free from zinc additions exhibits desirable characteristics of Weldability, castability and rollability not found in the zinc containing alloy. Commercially pure magnesium normally contains trace amounts of zinc. Incidental inclusion of zinc as an impurity from all sources should not exceed about 0.03 percent by weight of the total alloy.
There are two basic types of combination. The combination containing high calcium, in the range of about 0.3 percent by weight, and low aluminum, e.g., about 0.5 percent by weight, exhibits good ageability, high strength and excellent creep properties. Such alloy is most suitable Where the alloy is arbitrarily not to be brought to final shape or form by a cold working process, such as rolling, and high strength must be obtained by aging. Aluminum to calcium ratios in such combinations are less than about 2.6.
The other type combination contains low calcium in the range of about 0.15 percent by weight and high aluminum, e.g., about 1.2 percent by weight. This combination. offers higher ductility, and better castability, weldability without stress-relief, and good workability. Such alloy is most suitable where the alloy is to be cold worked whereby optimum strength is developed. Aluminum to'calcium ratios in such combinations are greater than about 2.6 and the sum of the percent of aluminum 3,370,945 Patented F eb. 27, 1958 ICC plus the sum of the percent of calcium is less than about 2.2 percent.
Increasing the calcium content beyond about 0.3 percent results in an alloy having better creep resistance and compressive yield strength, but generally results in poorer extrudability. However, more calcium may be used to advantage at higher aluminum levels for the purposes of preparing die castings and rolled sheet within the scope of the invention.
Manganese contents above about 1 percent impair properties, cause segregation, and tend to coarsen the cast grain structure. The alloy containing a manganese content below about 0.1 percent does not exhibit desired strength levels. Preferably the manganese content is in the range of 0.3 to about 0.8 percent.
Preferably the present alloy composition contains, by weight, from about 0.25 to abuot 1.5 percent of aluminum, from about 0.3 to about 0.8 percent of manganese, and from about 0.1 to about 0.4 percent of calcium, the balance being substantially commercially pure magnesium (purity about 99.8 percent).
Two especially preferred alloys have the following compositions, by Weight: 1) 0.5 percent of aluminum, 0.75 percent of manganese, 0.3 percent of calcium, and the balance magnesium, and (2) 1.25 percent of aluminuin', 0.50 percent of magnanese, 0.15 percent of calcium, and the balance magnesium.
The alloy may be made in the desired proportions according to the invention by melting together the alloy ingredients in proper proportions or by using hardeners of magnesium alloys containing the alloy constituents. In addition, the manganese may be added by direct reduction of manganese halide added to the flux.
Protection from oxidation during alloying is effected by the use of a magnesium chloride-free saline flux as in conventional alloying. The molten alloy may be flux refined by stirring the alloy with additional flux. The sorefined alloy is allowed to settle and may then be separated from the flux as by decanting into a suitable casting mold, as for example, a slab mold for rolling stock or a billet mold for extrusion stock. In the event the alloy is employed in die casting, the flux-refined metal may be decanted into the holding pot of the die casting machine.
The present alloy exhibits better creep resistance than the frequently used commercial alloy having the ASTM designation AZ91B.
The molten alloy of the invention is normally cast into either rolling slabs or extrusion billets. Usually the external surface of the cast piece is removed, as by a scalping operation. Extrusion billets are preheated to about 600-900 F. and are then die-expressed from a heated container. Rolling slabs are heated to about 700950 F. and reduced in thickness to about 0.1 inch sheet by multiple passes through the rolls of a mill, reheating the metal as necessary to avoid cracking.
The so-rolled metal sheet is then finished in a number of Ways as desired. The rolled metal may be annealed one hour at a temperature in the range of 700 to 950 F., quenched, and reduced by cold rolling at l to 2 percent per pass through steam heated rolls under conditions close to the cracking limit, and further annealedat a temperature in the range of 300 to 700 F. This method is particularly applicable to the present alloy having a relatively high aluminum to calcium weight ratio.
The rolled metal may also be finished by heating about one hour at 700 to 950 F., warm rolling the sheet to final thickness in one pass through the rolls of the mill, the metal exciting from the rolls at a temperature of 300 to 800 F., and quenching the exciting metal. If desired, the quenched metal may be aged or annealed at a temperature in the range of 300 to 800 F.
The alloy of the invention exhibiting a relatively low aluminum to calcium weight ratio is desirably and conveniently finished without further rolling upon solution heat treating the rolled metal at a temperature in the range of about 850 to 950 F., after which the metal is immediately quenched, and thereafter aged at a temperature of about 300 to 350 F.
Examples To illustrate the advantageous results which can be Car a purities, preheated to 600900 F. and ram extruded conventionally through a die while the metal and the container were at temperatures in the range of 500-800 F. Each alloy was extruded into a inch x inch strip at two different extrusion speeds, namely, 20 feet per minute, and a speed in the range of '70100 feet per minute. The so-obtained extrusions were aged 24 hours at 350 F. to bring the metal to the T5 temper condition and the extrusions were then subjected to mechanical testing. The results of these tests are shown in Table II.
achieved by the present invention, a series of composin TABLE II Properties, Extrusion at Composition, Percent by Weight 1 Test No. Al/Ca 20 fpm, 100 f.p.m.
Al Ca Mn Percent E CYS TS Percent E CYS TS 3 0. 17 0. 6 1. 8 12 16 37 12 15 39 0 3 0. 34 0. 6 0. 9 14 18 36 15 17 37 0. 0. 54 0. 6 0. 6 14 20 36 Hot short 0. 5 0. 2 0. 6 2. 5 8 15 40 16 40 0. 5 0 3 0. (5 1. 7 10 17 40 10 19 39 1. 0 0. 54 0. ti 1. 9 14 26 40 Hot short 1. 0 0.20 0. ti 5. 0 11 17 40 11 18 40 1.0 0. 13 0. 3 7. 2 10 39 11 15 39 1 Balance commercial purity magnesium. 2 Metal cracked on being extruded. I.p.m.=feet per minute.
tions according to the invention were prepared and cast into respective rolling slabs (e.g., 2" x 4" x 8" Each slab was treated as follows: the faces of the slabs were scalped to remove surface impurities or inclusions, the slab was heated to 700950 F. and reduced in thickness to about 0.1 inch sheet by multiple passes through the ro1ls of a mill, reheating the metal as necessary to avoid cracking. The rolled metal was then either annealed one hour at 950 F. and quenched, or, annealed for one hour at 700 F. Some of this metal was brought to a hard temper condition by cold rolling, at 1 to 2 percent per pass through steam heated rolls under conditions close to the cracking limit, and further annealing (one hour at 300 F). Some of the cold rolled metal was brought to the soft temper condition by annealing at 700 F., for one hour, instead of at 300 F. The s0-obtained metal in each of the hard temper and soft temper conditions was tested to determine the physical properties of the sheet. The results are listed in Tabie I.
In an additional test series, compositions according to the invention were prepared and cast both as extrusion stock and rolling stock. Extrusion stock was scalped and heated to a temperature in the range 600900 F. and extruded into inch x inch strip at 700 F. from a 3-inch container at a rate of from about to about 100 feet per minute. The so-obtained strip was aged 24 hours at 350 F.
Rolling stock was scalped and heated to a temperature in the range 700-950 F., then hot rolled starting with an initial temperature of 850 F., being reduced in thickness, by multiple passes through the rolls of a mill, from 2 inch to 0.1 inch. The so-obtained sheet was solution heat treated one hour at 950 F., water quenched and aged 24 hours at 320 F.
TABLE I Composition, Percent Physical Properties Test by Weight 1 Anneal No. Temp, Hard Temper Soft Temper Creep 2 at 300 F.,
I 5,000 p.s.i., 100 hrs., Al Ca Mn Percent E CYS TS Percent E CYS TS percent extension Additional compositions according to the invention were each prepare d and cast as a 3-inch diameter extrusion sheet wer billet. Each billet was scalped to remove surface im- CY S=cornpression yield strength in 1000's of pounds per square inch TS=ultirnate tensile strength in 1000's of pounds per square inch.
The so-obtained extrusion strip and these-obtained e each subjected to mechanical testing. The results of these tests are shown in Table III.
TABLE III T t N Composition, Percent by Weight 1 Properties, Extrusion at 50 f.p.m. Properties, Rolled Sheet Al Ca Mn Percent E CYS TS Percent E CYS TS 0. 5 0. 3 0. 25 14 10 34 lb 21 38. 5 0. 5 0. 3 0. 5 12 20 39 1 22 30, 5 0.5 0. 3 1. 0 12 19 3E) 10 20 38 1 Balance commercial purity magnesium.
metal was subjected to mechanical testing. The results 5 of these tests are shown in Table IV.
about 0.5 percent by Weight of aluminum, from 0.3 to about 0.8 percent by Weight of manganese, about 0.3 percent by Weight of calcium, and the balance substantially magnesium [free from zinc], the Weight ratio of aluminum to calcium being less than about 2.6 percent, and the alloy being characterized by good ageability without cold working.
TABLE IV Physical Properties Test Composition, Percent by Weight 1 Anneal, N0. Temp. F. Hard Temper Soft Temper Al Cu Mn Percent E OYS TS Percent E CYS TS 15 l. 0. 13 0. 3 700 26 36 16 14 35 1.0 0.13 0. 3 900 2 31 41 16 17 34 1.6 1. 0 0. 20 0.6 700 3 25 36 19 34 17 1. 0 0. 31 0. 6 700 3 26 37 19 15 3 1 1 Balance commercial purity magnesium.
Among the advantages of the alloy of the invention are that the alloy possesses the characteristic lightness of magnesium and the simultaneous combination of weldability without stress-relief, strength, workability, and low cost.
We claim:
1. The magnesium base alloy consisting essentially of from 0.1 to 1.75 percent by Weight of aluminum, from 0.1 to 1.0 percent by weight of manganese, from 0.05 to 0.6 percent by weight of calcium, and the balance substantially magnesium [free from Zinc], the combined total amount or aluminum and calcium in the alloy not exceeding 2.2 percent by weight.
2. The magnesium base alloy, as in claim 1, in which the Weight ratio of the aluminum content to the calcium content is less than about 2.6 percent.
3. The alloy, as in claim 1, in which the weight ratio of the aluminum content to the calcium content is greater than about 2.6 percent.
4. The magnesium base alloy consisting essentially of from 0.25 to about 1.5 percent by weight of aluminum, from 0.3 to about 0.8 percent by weight of manganese, from 0.1 to about 0.4- percent by weight of calcium, and the balance being substantially magnesium [free from zinc].
5. The magnesium base alloy consisting essentially of 6. The magnesium base alloy consisting essentially of 1.2 percent by weight of aluminum, from 0.3 to 0.8 percent by weight of manganese, about 0.15 percent by weight of calcium, and the balance substantially magnesium [free from zinc], the weight ratio of calcium to aluminum being greater than about 2.6 percent, and the alloy being characterized by weldability without stressrelief and by good cold workability.
References Cited CHARLES N. LOVELL, Primary Examiner.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0280708A1 (en) * 1986-08-21 1988-09-07 The Dow Chemical Company Photoengraving articles and methods of producing such articles
US4855198A (en) * 1986-08-21 1989-08-08 The Dow Chemical Company Photoengraving articles of zinc-free magnesium-based alloys
US6342180B1 (en) 2000-06-05 2002-01-29 Noranda, Inc. Magnesium-based casting alloys having improved elevated temperature properties
US20100198332A1 (en) * 2009-01-30 2010-08-05 Bodo Gerold Implant with a base body of a biocorrodible magnesium alloy

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB247149A (en) * 1925-02-05 1926-03-04 Gilbert Michel Improvements in manufacture of magnesium and its alloys
US1720436A (en) * 1926-11-13 1929-07-09 Ig Farbenindustrie Ag Process of refining magnesium and its alloys
US2185452A (en) * 1937-09-01 1940-01-02 Magnesium Dev Corp Method of heat treating magnesium base alloys
US2185453A (en) * 1937-09-01 1940-01-02 Magnesium Dev Corp Method of heat treating magnesium base alloys
US2314024A (en) * 1942-03-23 1943-03-16 Dow Chemical Co Magnesium base alloy
GB658707A (en) * 1949-05-09 1951-10-10 Dow Chemical Co Method of improving magnesium and its alloys
US2620270A (en) * 1950-04-03 1952-12-02 Dow Chemical Co Method of improving magnesium and the binary magnesium-base alloy of magnesium and manganese
US2671039A (en) * 1946-05-02 1954-03-02 Bendix Aviat Corp Magnesium die casting alloy and process
US3146096A (en) * 1962-11-23 1964-08-25 Dow Chemical Co Weldable high strength magnesium base alloy

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB247149A (en) * 1925-02-05 1926-03-04 Gilbert Michel Improvements in manufacture of magnesium and its alloys
US1720436A (en) * 1926-11-13 1929-07-09 Ig Farbenindustrie Ag Process of refining magnesium and its alloys
US2185452A (en) * 1937-09-01 1940-01-02 Magnesium Dev Corp Method of heat treating magnesium base alloys
US2185453A (en) * 1937-09-01 1940-01-02 Magnesium Dev Corp Method of heat treating magnesium base alloys
US2314024A (en) * 1942-03-23 1943-03-16 Dow Chemical Co Magnesium base alloy
US2671039A (en) * 1946-05-02 1954-03-02 Bendix Aviat Corp Magnesium die casting alloy and process
GB658707A (en) * 1949-05-09 1951-10-10 Dow Chemical Co Method of improving magnesium and its alloys
US2620270A (en) * 1950-04-03 1952-12-02 Dow Chemical Co Method of improving magnesium and the binary magnesium-base alloy of magnesium and manganese
US3146096A (en) * 1962-11-23 1964-08-25 Dow Chemical Co Weldable high strength magnesium base alloy

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0280708A1 (en) * 1986-08-21 1988-09-07 The Dow Chemical Company Photoengraving articles and methods of producing such articles
EP0280708A4 (en) * 1986-08-21 1988-12-15 Dow Chemical Co Photoengraving articles and methods of producing such articles.
US4855198A (en) * 1986-08-21 1989-08-08 The Dow Chemical Company Photoengraving articles of zinc-free magnesium-based alloys
US6342180B1 (en) 2000-06-05 2002-01-29 Noranda, Inc. Magnesium-based casting alloys having improved elevated temperature properties
US20100198332A1 (en) * 2009-01-30 2010-08-05 Bodo Gerold Implant with a base body of a biocorrodible magnesium alloy
US8268235B2 (en) * 2009-01-30 2012-09-18 Biotronik Vi Patent Ag Implant with a base body of a biocorrodible magnesium alloy

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