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TECHNICAL REPTO , 0. WAL-TR--323.4/

DTlC'1EILECTEg

RANK L. ARR

0.DATE OF ISSUE - DECIUM 1461

ONS CODE 5010.,.84o20051RESEARCH OF METALS AND NONMETALLIC MATERIALS FOR ORDNANCE CONSTRUCTION

D/A PROJECT 5993-32-002

Th5is documet hasbe prvfor public reloase and s=ale; ibgdistribution is unlmited.

,. 1 WATERTOWN .72p MASS. IV,

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3 ASTIA AVAILABILITY NOTICEI Qualified requesters may obtain copies of this report from ASTIA.

Copies available at Office of Technical services $0.75.

DISPOSITION INTRUCTIONIS

Destroy; do not return

1N

AD Steels, stainless -

mechanical properties

Titanium

LOW TEMPERATURE MECHANICAL PROPERTIESI OF 300 SERIES STAINLESS STEELS AND TITANIUM

Technical Report No. WAL TR 323.4/1

By

Thomas S. DeSisto

andIdFrank L. Carr

Date of Issue - December 1961

OMS Code 5010.11.8420051Research of Metals and Nonmetallic Materials for Ordnance Constr',ction

D/A Project 5B93-32-002

K' -n For

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WATERTOIN ARSENAL oWATERTOWN 72, MASS. iki

- .- f

WATERTOWN ARSENAL LABORATORIES

TITLE

LOW TEMPERATURE MECHANICAL PROPERTIESOF 300 SERIES STAINLESS STEELS AND TITANIUM

ABSTRACT

-A tensile test cryostat is described for the temperature range-240 F to -452 F, which consists of a temperature recording and controlsystem, and a diameter measurement system which includes a scanning con-~trol system. True stress-strain properties of the 300 series stainless

steels and iodide and conmiercially pure titanium were obtained from roomtemperature to -452 F. Serrated load-elongation curves obtained at-452 IF and the sequence of deformation in multi-necked specimens at thistemperature are discussed.

THOMAS S. DeSISTOGeneral Engineer

FRANK L. CARIL

Materials Engineer

APPROVED:

REPORT APPROVED.F. LLVAN

D rector Date. 6/tertown Arsenal Laboratories WAL Board of Review

Chairman..-

*1

ABSTRACTCONTENTS

Page

INTRODUCTION.... 9.... . .................... 3

MATERIALS AND PROCEDURE .. . . .... .. .. . .. .. . ... 3

Materials, Chemical Analysis and H-eat Treatment . . . . . . . 3Testing Procedure. .... ... #. .* .0. .*.... *... 3

TensileTestCrystat . .. . . ... . ... .. .. . . .

TEST RESULTS .. . ... . . . . . . . . . . . . . . 7

300 Series Stainless Steels .. .. . ... ... . . . . 8

Titanium . . . . .. .. . . . . . .* . . . . . . . . 9Serratd Loa-Elongation Curves......... .*** 9

ILUSTR.ATIONS . . . . .. .. . .. ... . . . . . . 13

RE FERENCES. .. ... ......... .... . . . . . . . . . . . 32

INTRODUCTION

The use of liquefied gases in electronic devices and missile propel-

lant bystems, and the extremely low temperatures which are encountered inouter space, have created a demand by design engineers for mechanicalproperty data of engineering materials at cryogenic temperatures.

'While recently, considerable effort has been devoted to obtainingtensile and other mechanical properties of engineering materials at cryo-genic tempevatures, instantaneous diameter measurements during tensiletesting have not been attempted.

Recognizing the importance of the true stress-strain test and theneed for specimen diameter measurements in tests where the material de-forms by a series of discontinuous yields, Watertown Arsenal Laboratoriescontracted with A. D. Little, Inc. to construct a tensile test cryostatcapable of measuring and recording instantaneous diameter data.

The purpose of this report is threefold:

a. To describe briefly the tensile test cryostat.

b. To present engineering and true stress-strain data obtained withthis equipment on the 300 series stainless steels and commercially pureand iodide titanium.

c. To comment on observations noted on the formation and developmentof necks at -452 F.

MATERIALS AND PROCEDURE

Materials, Chemical Analysis and Heat Treatment

The materials used in this investigation together with the specimennomenclature and chemical analysis are shown in Table I. The stainlesssteel and commercially pure titanium were utilized in the as-receivedmill-annealed condition. The iodide titanium was annealed five hours at1600 F in a vacuum.

Testing Procedure

Round 0.252-incl. diameter tensile specimens, as shown in Figure 1,were used in this testing program. Tests were condr'cted in a Baldwin60,000-pound hydraulic testing machine at a controlled platen speed of

* 0.01 inch per minute. Low temperature tests at -105 F, -240 F and -320 Fwere conducted in a double-walled metal container. The coolants usedwere alcohol, with dry ice added, for -105 F; isopentane in the inner con-tainer with liquid nitrogen added to the outer container, when needed,for -240 F; and liquid nitrogen at its boiling point, -320 F. Over this

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temperature range, an instantaneous diameter gage 2 was used to obtaindiameter data for true stress-strain calculations. For tests at -452 F,liquid helium was used in the tensile cryostat.

Tensile Test Cryostat

The tensile test cryostat consists of a low-temperature tensile testchamber, a temaperature recording and control system, and a tensile diametermeasurement system which includes a scanning control system. The unit wasdesigned to be compatible with an existing true stress-strain computer.

3

A schematic diagram of the test apparatus is shown in Figure 2. The low-temperature test chamber, designed for the temperature range of -240 F to-452 F, consists of an inner vessel which contains the cooling medium andwhich comprises the actual test volume to be maintained at the desiredtest temperature. The inner chamber is surrounded in turn by a vacuumjacket, a liquid nitrogen bath and outside vacuum jacket.

I The test chamber is supported by the lower head of the testing ma-chine; the upper head moves relative to the lower head.

Both top and bottom specimen holders are sealed in the cryostatagainst leakage by removable "0" rings at the ambient ends. The topholder, together with the four diameter-measuring caliper fingers, passthrough the cover plate into the test volume through the top of the testchamber, and are part of the measuring-head assembly. The specimenholders were designed to withstand 20,000 pound loads.

The approximate coolant consumption rates for a test at -452 F are asfollows:

Nitrogen consumption:

precooling loss 3.0 liters

heat-leak loss 0.5 liters per hour

Helium consumption:

precooling loss 4.6 liters

heat-leak loss 2.0 liters per hour

The temperature in the test chamber is measured by four copper-constantan thermocouples, one at each end of the four caliper fingers.The thermocouples are connected in series to increase the output signal.The temperature-controller consists of a Leeds and Northrup potentiometerand duration-adjusting type (D.A.T.) controller. The cooling liquid istransferred from a storage Dewar flask to the test volume through a vacuumjacketed helium transfer tube when the solenoid valve connected to thehelium exhaust tube of the test chamber is opened on a signal from a relay

controlled by the D.A.T. unit.

-5-

- 4

The diameter-measurement system consists of four caliper fingersspaced at 90 degrees around the 0.252-inch diameter specimen in a planeperpendicular to the specimen axis. The fingers are coupled each to alinear variable differential transformer through a pivoted right anglearm, and are each held against the test specimen by the unbalanced mass ofthe right angle arm.

The output signal, which is proportional to the average diameter ofthe speciy,.en, is fed into the true stress-strain computer and can be readvisually on a graduated dial or, when used in conjunction with load datafrom the testing machine, can provide an autographic curve of true stress-strain on a Baldwin MD-2 recorder. If desired, diameter profile datacan be obtained on an auxiliary recording system.

A scanning motor mounted on the cover of the test chamber drives thecarriage carrying the four caliper fingers over the gage length of thespecimen seeking a minimum diameter. An arm, which is friction coupledto the graduated diameter dial of the computer, serves as a memory device.Once minimum diameter is obtained, the fingers scan until a diameter 0.001inch greater than minimum diameter is obtained, thqn the direction of scanis reversed on a signal from a microswitch, and the motor drives thefingers back through minimum diameter to a diameter 0.001 inch greater,and then the scan is again reversed. Provision is mde for a full gagelength scan to study the development of multiple necks. Limit switchesare provided to prevent travel of the fingers beyond the shoulders of thespecimen.

Records of loads and platen displacement were made on a Baldwin MD-2recorder, with loads obtained from the testing machine Bourdon tube micro-former and displacement measured by a deflectometer. The deflectometer,placed under the moving platen, was capable of strain read-outs of 0.036inch per inch of chart displacement. The full range of the unit was

0.5 inch.

After the specimen was mounted into the test chamber and cooled tothe desired test temperature, the diameter-indicating dial was adjustedto read the calculated diameter at the test temperature. This wasnecessary as contraction of the four caliper fingers could indicate a

false diameter reduction. For tensile tests, where load displacement re-cords were obtained, the specimen gage length was scanned before and aftereach serration and the minimum diameters of the several necks were notedand recorded on the curve.

True stress data were obtained by dividing the area of the specimenat the time of the serration into the peak load. These data thereforereflect the upper envelope of the flow stress curve.

-6-

TEST RESULTS

The data obtained in this investigation are plotted in Figures 3through 19 and tabulated in Table II.

TABLE II

TENSILE PROPERTIESUltimate True

Testing Tensile Elon- Reduction Stress at Fracture TrueTemp Strength gation of Area Max. Load Stress Strain at Fracture

(deg F) (psi) (%) (%) (psi) _(psi) Max. Load Strain

AISI 302 Stainless Steel

R.T. 94,400 75.0 80.7 149,600 319,550 0.460 1.647-105 152,400 52.5 73.7 218,700 368,850 0.362 1.338-240 191,300 48.0 71.7 262,900 422,300 0.318 1.264-320 219,300 46.0 69.5 292,150 481,150 0.286 1.183-452 249,500 41.0 54.8 548,500 550,900 0.787 0.794

AISI 303 Stainless Steel

R.T. 100,200 59.0 67.4 157,800 255,000 0.452 1.319-105 161,500 43.0 56.8 219,900 299,000 0.299 0.847-240 206,300 37.0 53.6 266,000 355,200 0.254 0.762-320 234,100 35.0 51.5 293,500 398,500 0.227 0.718-452 266,500 29.6 37.0 423,600 423,600 0.462 0.462

AISI 304 Stainless Steel

R.T. 95,100 65.0 83.4 154,100 330,100 0.482 1.789-105 151,100 55.0 77.0 211,800 387,900 0.336 1.467-240 193,800 46.0 73.9 264,200 447,000 0.308 1.339-320 221,400 46.5 71.8 301,800 488,000 0.308 1.263-452 242,500 39.0 49.8 363,400 478,100 0.402 0.687

AISI 316 Stainless Steel

R.T. 93,900 47.0 77.5 133,900 269,700 0.355 "1.484-105 131,500 59.0 78.0 198,800 369,000 0.442 1.517-240 161,10O 6o.o 77.7 256,000 435,000 0.462 1.500-320 184,300 59.0 76.2 270,500 497,400 0.384 1.434-452 216,400 52.0 59.7 360,200 530,250 0.508 0.907AISI 347 Stainless Steel

R.T. 99,300 50.0 73.0 143,200 266,000 0.365 1.300

-105 136,600 53.0 72.2 194,700 326,000 0.355 1.378

-240 172,100 48.0 67.4 238,600 374,400 0.327 1.119-320 201,400 46.0 65.5 274,500 423,800 0.308 1.o65-452 236,400 38.0 54.7 438,000 500,300 0.593. 0,789

A-55 Titanium

R.T. 68,700 30.0 50.1 77,200 111,300 0.120 0.692-105 87,500 39.5 60.8 109,100 181,200 0.217 0.934

-240 107,200 58.5 70.7 157,700 254,600 0.384 1.225

-320 139,000 53.5 69.5 200,900 313,400 0.365 1.184-452 176,500 37,0 55.8 298,700 353,500 0.520 0.771

Iodide Titanium

R.T. 46,000 61.0 81.5 67,000 144,100 0.374 1.691-105 72,000 57.0 84.3 102,100 198,700 0.346 1.856

-240 92,400 67.0 88.0 , 138,700 289,000 0.403 2.120-320 112,000 72.0 78.2 185,500 290,000 0.503 1.521-452 143,200 57.5 61.6 247,100 320,400 0.545 0.957

-7-

300 Series Stainless Steels

The tensile strengths of the 300 series stainless steels, plotted inFigure 3, generally increase with decreasing temperature. This increaseis fairly linear to -320 F, but at -452 F the strengths of types 302, 303and 304 are lower than would be expected by extrapolating from the highertemperatures. This might be taken to indicate a slight degree of em-brittlement at -452 F.

The ductility of the stainless steels tested generally decrease withdecreasing temperature. An exception is Type 316 which increases fromroom temperature to -105 F, remains constant to -320 F and drops at-452 F. The least ductile of these materials is Type 303, which has thehighest tensile strength.

Tnear plots of true stress-strain for the temperature oange investi-

gateCd re plotted in Figures 4 through 8. At the higher strains, the Aflow .3ress increases with decreasing temperature. .At the lower strains,the nature of the curves are different. In the vicinity of 0.15 to 0.17strain, the flow stress of Types 302, 303, and 304 is lower at -452 F thanat -320 F. Over the same range of strain, the stress of Type 347 at-452 F is coincident to the flow stress curve at -320 F. It is alsonoted that, at -105 F and below, there is a concave upward trend in thecurve in this strain range.

Tis increased rate of strain hardening has been explained by Powell,et al, to be caused by the strain-induced transformation of rezainedaustenite to martensite. It is observed also that the concave upwardtrend is not evident in Type 316. This is surprising, as X-ray analysis,~of the fractured specimens indicated considerable transformation of re-

*tained austenite in the threaded and deformed portions of the specimenstested at -452 F. The results are as follows:

7 IRetained Austenite %

Specimen Threads Shank at Fracture

302 100 0304 100 1.9316 100 11.4347 100 8.0

True stress at maximum load for the 300 series stainless steelsplotted in Figure 9 increases with decreasing temperature to -320 F andthen increases more markedly. This marked increase at -452 F is attri-

buted to the deformation process, which rasults in a higher strain atmaximum load. The fracture stress, shown in Figure 9, also increases withdecreasing temperature. An exception is Type 304 which shows a slightdecrease below -320 F.

Strain at maximum load, plotted in Figure 10, generally decreaseswith decreasing temperature to -320 F and then increases sharply. An

-8-

Won

exception is Type 316 which increases from room temperature to -240 F,decreases at -320 F and increases sharply at -452 F. This increase instrain at maximum load below -320 F can be explained by the fact that at-452 F the deformation process is not continuous at any onu location andthe metal can tolerate a much higher strain before maximum load is reached.

Titanium

The tensile strengths of the commercially pure (A-55) and iodidetitanium, plotted in Figure 11, increase approximately 155% and 210%respectively, from room temperature to -452 F. Over the same temperaturerange, ductility, as measured by either percent elongation or percentreduction of area, increases from room temperature to either -240 F or-320 F and then decreases at -452 F. It is noted that the ductility of theA-55 material is greater at -452 F than at room temperature. This be avioris common with metals of high purity. In the case of titanium, Guard9 hasshown that the operative deformation mechanisms are dependent upon puritylevel as well as temperature.

Linear plots of true stress-strain for the temperature range inves-tigated are shown in Figures 12 and 13. Strain at maximum load "M" andfracture strain "F" are noted on each curve. The flow stress of both theA-55 and iodide titanium increases with decreasing temperature.

True stress at maximum load and fracture stress, plotted in Figure 14,increase with decreasing temperature. Of interest is the comparison ofthese curves over the full temperature range. While the stress at maximumload is greater for the A-55 material over the full temperature range, thefracture stress of the iodide titanium is greater from room temperature to-240 F, but is less at the lower temperature.

True strain at maximum load for the A-55 and iodide titanium, plottedin Figure 15, generally increases with decreasing temperature. This in-crease coincided with the gradual change in reformation mechanism frompredominantly slip to a mixture of slip and twinning at the lower temperatures.

Serrated Load-Elongation Curves4Tensile stress-strain curves at elevated temperatures often show loadserrations, due to strain aging. Similar serrations are evident in tests

below -320 F where a different mechanism must be opeatiye. The reasonsadvanced for these serrations are many and varied. , ,74 There has not,however, been any attempt to measure instantaneous diameter changes whilethe specimen is deforming by a series of discontinuous yields.

A typical load-elongation curve for a specimen of 302 tested at-452 F is shown in Figure 16. In this plot, the numbers above the loadserrations represent the average diameter of one or several necks at theindicated load. The lowest set of figures represent the diameter of thefirst neck to form and the subsequent figures represent the additional

-9-

Po

*L necks as they formed. For this specimen the first neck formed in thelower third of the gage length, the second neck formed in the middle andthe last neck formed in the upper third of the gage length. As indicatedon the plot, - ,e specimen fractured at the first neck formed.

This pattern of events was not the general rule, however, as oftenthe first neck formed in the middle or upper third of the gage length andthe specimen fractured at one of the later forming necks. While not notedon the plot, the diameters between the necks were from 0.008 to 0.020 inchgreater than the noted diameters. It was also observed that in theportion of the curve where there are two or more necks, load serrationscan be accompanied by deformation in a single neck, two necks simultaneouslyor neither of the necks. In the last case deformation takes place elsewherealong the gage length.

The serrated load-elongation curve for a specimen for Type 316 isshown in Figure 17. It is evident that small serrations begin after con-siderable plastic flow and then grow in magnitude with increasing stressuntil fracture occurs. It is also evident that the last full serrationis much larger than the preceding serrations and wasaaccompanied by largelocal deformation.

The serrated load-elongation curve for a specimen of commerciallypure titanium is shown in Figure 18. In this plot the first load serra-tion appears to originate from the elastic portion of the curve. Theserrations increase in magnitude with increasing stress until fractureoccurs. Again, as with Type 316 the last full serration is much largerthan the preceding serrations and was accompanied by large local defor-mation. It is noted that the first 30 serrations resulted in a diameterreduction from 0.252 to 0.222 inch, with each serration accompanied byapproximately 0.001 inch diameter change.

The serrated load-elongation curve for a specimen of iodide titaniumis plotted in Figure 19. The first serration appears to originate from

the elastic portion of the curve and is followed by two others of equalmagnitude. Following these initial serrations is an extended portion ofstrain without serrations which is in turn followed by additional serrations.These additional serrations are preceded by decreasing portions of plasticstrain as the serrations increase in magnLtude to fracture. This is incontrast to the results for the commercially pure titanium and the stain-less steel, where no visible plastic strain occurred except during theload drops. Again, as in previous cases, there is a large characteristicserration immediately preceding fracture. It is assumed that during thisserration, an internal crack has formed at some inclusion or otherwise,as the specimen fractures on the elastic portion of the next load cyclewith no apparent diameter change.

-10-

SUMMARY

The mechanical properties of the 300 series stainless steels andcommercially pure and iodide titanium have been determined from room

*temperature to -452 F. A tensile cryostat used to obtain the mechanicalproperty datA at -452 F was described. True strain at maxmum load forthe A-55 and iodide titanium increase with decreasing temperature. Thisincrease coincides with the change in deformation mechanism from pre-dominantly slip to a mixture of slip and twinning at the lower tempera-tures. Bj contrast, strain at maximum load for the 300 series stainlesssteel generally decreased with decreasing temperature to -320 F, butincreased markedly at -452 F. This marked increase can be explained bythe fact that at -452 F the deformation process is not continuous at anyone location and the metal can tolerate a much higher strain before maxi-

* mum load is reac'ed.

All materials tested in this investigation deformed by a series ofdiscontinuous yields at -452 F. Load serrations were accompanied by de-formation in a single neck, two necks simultaneously or elsewhere -alongthe gage length. The shape of the serrated load-elongation curve variedwith the material. For the 300 series stainless steels, serrations beganafter consideiable plastic strain while for both the A-55 and the iodidetitanium the first serration appears to originate from the elastic portionof the curve. However, all specimens tested which fractured beyond maxi-mum load had a large characteristic serration immediately preceding frac-ture. This serration was accompanied by large local deformation. As thespecimens fractured on the next load cycle with no apparent diameterchange, it is assumed an internal crack has initiated at some inclusionor otherwise during this serration.

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TRUE STRESS-STRAIN CURVES OF AI$1 38STAINLESS STEEL AT VARIOUS TEMPERATURES

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REFERENCES

1. A. D. LITTLE, INC., Design, Development and Fabrication of One Low~Temperature Test Ot.amber with Instantaneous Diameter Masurement

Device, Final Technical Report, Contract DA-19-O20-505-ORD-4642,30 January 1960.

2. NUNES, J., and LARSON, F. R., A Method for Determining the PlasticFlow Properties of Sheet and Round Tensile Specimens, WatertownArsenal Laboratories, WAL TR .1/1, MIarch 1061.

3. DeSISTO, T. S., and DRISCOLL, D. E., True-Stress True-Strain Computer,Watertown Arsenal Laboratories, WAL TR 111/23-1, March 1957.

' 4. POWEI1,, G. W., MARSHALL, E. R.., and BACKOFEN, W. A., Strain Hardeningof Austenitic Stainless Steels, Transactions, ASM, v. 50, 1958,

5. GUARD, R. W., Low Temperature Tensile Properties of Titanium; rfect

of Annealing Temperature, General Electric Company, Report No. 55-RL-1339,Contrct AF-33(616)-2120, July 1955.

6. SMITH, R. L., and RUTHERFORD. J. L., Tensile Properties of ZoneR _PReined Iron in the Temperature Range from 298 K to 4.2 K, Transactions,

{ I1AIE, v. 209, July 10957. p. 857.

"7. WESSEL, E. T., Metals at Low Temperatures, Transactions, ASM, v. 49,.1957s p. 149.

•8. EIDEN, A. S., and COLLINS, S. C., Fracture and Yield of 1020 Steel at

Low Temperatures, Journal of Applied Physics, American Institute ofPhysics, v. 22, no. 12, October 1951, p. 1296.

-32-

WATERTOWN ARSENALWATERTOWN 72, MASSACHUSETTS

TECHNICAL REPORT DISTRIBUTION

r Report No.: WAL TR 323.4/1 Title: Low Temperature Mechanical Proper-December 1961 ties of 300 Series Stainless Steels

and TitaniumDistribution List approved by Ordnance Materials Research Office,

1 December 1960.

No. of

1 i Director, Army Research Office, Department of the Army,

Washington 25, D. C.

Commanding Officer, U. S. Army Research Office (Durham), Box CM,Duke Station, Durham, North Carolina

1 ATTN: ORDOR-EDJ1

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1 ATTN: Dr. G. H. Reisig

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* Commanding General, Ordnance Weapons Command, Rock Island, Illinois1 ATTN: ORDOW-IX2 ORDOW-TX

1 Commanding General, U. S. Army Ordnince Special Weapons AmmunitionCommand, Dover, New Jersey

Commanding General, U. S. Army Rocket and Guided Missile Agency,Redstone Arsenal, Alabama

1 ATTN: ORDAB-DV5 ORDXR-RGA, Mr. R. L. Wetherington1 ORDXR-RMO, Lt. E. J. Wilson

No. ofCopies TO

Commanding Officer, Detroit Arsenal, Center Line, Michigan1 ATTN: ORDMX-BMW1 ORDMX-AL

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1 ATTN: ORDTL .012, Technical Reference Branch j1Commanding Officer, Frankford Arsenal, Philadelphia 37, Pennsylvania

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Commanding General, Corps of Engineers, Fort Belvoir, Virginia1 ATTN: Eng. R&D Laooratories

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chief, Bureau of Naval Weapons, Department of the Navy, Room 2225,Munitions Building, Washington 25, D. C.

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Energy Commission, Washington 25, D. C.

National Aeronautics and Space Administration, 1520 H Street, N. W.,

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Director, Jet Propulsion Laboratory, California Institute ofTechnology, Pasadena 3, California

1 ATTN: Dr. L. Jaffe

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British Joint Services Mission, 1800 K Street, N. W.,Washington, D. C.

4 ATTN: Technical Services Department

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