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AD266 896

ARMED SERVICES TECHNICAL INFORMATION AGENCYARLINGTON HALL STATIONARLINGTON 12, VIRGINIA

UNCLASSIFIED

I

NOTICE: When government or other drawings, speci-fications or other data are used for any purposeother than in connection with a definitely relatedgovernment procurement operation, the U. S.Government thereby incurs no responsibility, nor anyobligation whatsoever; and the fact that the Govern-ment may have formilated, furnished, or in any waysupplied the said drawings, specifications. or otherdata is not to be regarded by implication or other-wise as in any manner licensing the holder or anyother person or corporation, or conveying any rightsor permission to manufacture, use or sell anypatented invention that may in any way be relatedthereto.

MELLON INST'ITUTE00

Quarterly Scientific Progress Report

Report No. 14for the period

August 1, 1961 - October 31, 1961

C.>

STRESS CORROSION OF HIGH STRENGTH STEELS

AND ALLOYS; ARTIFICIAL ENVIRONMENT

x E: Rox ,"•I5L

Research Project No. 389-2 DEC I te

TtPDR _._ i

Sponsored by

U. S. Army Ordnance, Frankford Arsenal

Mr. H. Rosenthal, Contract Monitor

Contract No. DA-36-034-ORD-3277RD

Approved 46'-I Dr. H. T- AnthonyStaff Adviser

MELLON INSTITUTE

Report No. 14

QUARTERLY SCI ENTI FIC PROGRESS REPORT

for the period

August I, 1961- October 31, 1961

STRESS CORROSIONOF HIGH STRENGTH STEELSAND ALLOY S; ARTIFIC IA L ENVI RONMENT

Research Prcoject No. 389-2

Sponsored byU. S. Army Ordnance, Frankford Arsenal

Mr. H. Rosentha i, Contract Monitor

Contract No. DA-M-034-ORD-3277RD

This Report Presented By TheProja ct Staff

C. 3J. Ovven, FellowW. D. Ruble, Lesearch Assistant

The publication of this report does aqot necessarily constitute approvalby the Army of the findings or concdasions contained therein.

Nor|

TABLE OF CONTENTS

Page

ABSTRACTaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaaa- ii

I. INTRODUCTION------------------------------------1

II. EXPERIMENTAL PROCEDURES

Test Methods------.......-.......... zApparatus ------------------- ------ zAlloy Sample Material ------------------------- 3Sample Preparation --------------------------- 4Sample Testing -------------------------------- 5Status of Sample Material ---------------------- 5

III. EXPERIMENTAL

Sample Preparation and Heat Treatment 6Stress Corrosion Testing ---------------------- 7

Bent Beam Tests ----------------------- 8U-Bend Tests --------------------------- 10

IV. FUTURE WORK ----------------------------------- 13

II

ABSTRACT

Stress corrosion test methods, apparatus, high strength

alloy sample material for testing, sample preparation, sample testing,

and present status of sample material are presented in brief.

Available heat treatment data for the PH15-7Mo, Vascojet

1000, D6Ac, and B12OVCA alloys, heat treated to the approximate

required strength levels of Z00, 220, 240 Kpsi and maximum Y.S. (150,

170, and maximum for the titanium alloy) are given. Data for the

remaining alloys, including 300M and Rocoloy 270 are in process.

Cumulative stress corrosion test data for the various bent beam

and U-bend tests are presented. Included are bent beam data for 4137

Co and AM355 alloys, and U-bend data for AM355, PHI5-7Mo, B12OVCA,

4137 Co, and Ardeform 301. Indicated probability of proneness of these

alloys to stress corrosion is discussed for each in accordance with

the data presented.

ii

I. INTRODUCTION

The project work described herein represents a portion of

a grant made available by the Army to promote a general scientific

advancement in the area of case materials for missiles. This specific

paloject is concerned with the synthetic environment stress corrosion

testing of specified high strength steels and alloys. The research

objectives of the project were presented in Report No. 1.

Natural environmental tests on high strength steels and alloys

are being conducted by Aerojet General Corporation, with actual produc-

tion environments and rocket proDellant environments being utilized. By

prior mutual agreement, the same steel and alloy sheet material will be

used for both projects and possible heat treatment variations will be

circumvented by exchanging heat treated material whenever possible.

A number of drawings and schematic diagrams of apparatus

and test methods pertinent to the project have been presented in prior

reports. In addition, surveys of applicable industrial and military

literature have also been presented previously (Reports 2 and 3).

This report presents further information on continuing

U-bend and bent beam tests for the assigned alloys, and for Rocoloy

270, 4137 Co, and Ardeform 301 missile steels.

2.

II. EXPERIMENTAL PROCEDURES

Test Methods

A discussion of the U-bend and bent beam test methods

together with an outline of the synthetic stress corrosion test environ-

ments used in performing the research are given in the July, 1960,

Monthly Scientific Report, Report No. 1.

All recently-exposed (and future) samples being subjected to

stress corrosion testing are being weighed prior to exposure to the test

solutions to provide, whenever possible, general corrosion information.

Apparatus

Schematic drawings of bent beam sample holders, the U-bend

test and holders, a sample bending device for bent beam specimens, and

a stress corrosion test tank were presented in Report Nos. 1 and 3.

Polyethylene containers are presently being used for the

stress corrosion exposure of U-bend specimens to the various synthetic

environments. Each container will adequately hold six U-bend specimens.

The use of these containers will supplement the sample testing presently

being conducted in epoxy-coated tanks.

Construction of shelving and an aeration system (Report No.

6) together with other pertinent items has facilitated (wherever feasible)

3.

the transfer of samples under test from the glass containers to the

epoxy-coated test tanks. The completed facility is illustrated in

Report No. 7.

Alloy Sample Material

The alloys being used in the study on stress corrosion

inciude:

1. Low Alloy: Ladish D6Ac.

2. Si-Modified 4300 Series: 300 M.

3. Hot-Worked Die Steel: Vascojet 1000.

4. Cold-Worked PH Steel: AM 355.

5. Heat-Treated PH Steel: PHi5-7Mo.

6. Titanium Alloy: B12OVCA.

7. Low Alloy-Cobalt Modified: 4137 Co.

8. Low Alloy-Cobal Modified: Rocoloy 270.

9. Stretch-Formed 1 7/7 Stainless Steel: Ardeform 301.

All of the sample material is being tested in sheet form

and was procured as such.

Chemical analyses for the above listed alloys and for the

comparative heats are given in their entirety in Table I in Report No.

13. Physical properties and heat treating surveys for the alloys were

presented in Report No. 12.

rIbU

4.

Sample Preparation

Sheet material of the various alloys was sheared into

slightly over-size U-bend, bent beam, and tensile specimens in both

the primary (direction of lowest Y.S. ) and secondary directions. The

specimens were then wet-ground to width, length, and thickness (if

necessary). Sampple thickness was maintained between 30 and 50 mils,

and as close to 50 mils as possible.

After heat treatment surveys were conducted (see Report

No. 12) to determine the Y. S. variation with tempering temperatu~re

for each alloy (not necessary for AM 355), the specimens were heat

treated to strength levels approximating 200, 220, 240 Kpsi and maximum

Y.S. Heat treating of the BlZOVCA alloy consisted of aging in an inert

atmosphere (see Report No. 12).

All the surfaces except the ends of the heat treated specime-xs

were then polished with emery paper to remove oxide films, the final

polish being administered with 240-grit emery. Care was taken to assure

a uniformly square edge on the specimens. A tendency of the D6Ac,

V-1000, and 300 M specimens to decarburize was circumvented by

carefully wet-grinding the surfaces of the heat-treated samples an

additional 5 mils per surface.

5.

Sample Testing

The U-bena specimens were bent into a V-shape with a special

bending apparatus, sprung into clips (see Report No. 12). and immersed

in each of the five test solutions (one-molar NaCI, Na 2 SO 4 , NaNOy3

NaPO3 . and Na 2 S).

The bent beam specimens were precision-cut to length and

sprung into a holder with a bending device (see Report No. 12).

Status of Sample Material

The present status of the alloy sample material to date:

1. D6Ac - heat treatment incomplete.

2. 300M - heat treatment incomplete.

3. Vascojet 1000 - heat treatment incomplete.

4. AM 355 - all U-bends and some bent beam samples

under test.

5. PHl5-7Mo - all U-bends but no bent beam samples

under te s t.

6. B12OVCA - heat treatment incomplete.

7. 4137 Co - under test.

8. Rocoloy 270 - undergoing final machining.

9. Ardeform 301 - under test.

-

6.

MI. EXPERIMENTAL

Sample preparation, heat treatment, and stress corrosion

testing of all alloys noted in the previous section of this report are

continuing.

1. Sample Preparation and Heat Treatment

During the period of this report, the PH15-7Mo, Vascojet

1000, D6Ac, and B1ZOVCA U-bend and/or bent beam stress corrosion

specimens were heat treated to the approximate strength levels required.

These Y.S. level objectives were Z00, 220, Z40 and maximum Kpsi for

the first three of the above and 150, 170, and Z00 Kpsi for the B12OVCA

material. Heat treatment schedules were in accordance with the

information presented in the heat treatment surveys (see Report No. 12)

for these alloys.

While all heat treating (including 300M) is not as yet com-

plete, the available tensile results for a number of these alloys are

presented in Tables I (PHl5-7Mo), II (Vascojet 1000), and III (D6Ac).

The Y.S. level objectives of 200, 220, 240 and maximum Kpsi were not"

precisely obtained but the range of values is sufficient for test purposes.

In addition, the Y. S. differential for the same tempering temperature in

the two test directions (primary and secondary) was somewhat greater

than was anticipated in some case&.

k

7.

Photomicrographic work for the various as-received and

heat treated alloys is incomplete and will be presented in the following

irepaort.

A considerable number of heat treated U-bend and bent

beam samples are undergoing final surface preparation and it is expected

that test data for same will also be presented in the next report.

2. Stress Corrosion Testing

The remainder of the as-received B12OVCA U-bend samples

and all of the heat-treated PIH5-7Mo U-bend samples have been sub-

jected to testing during the report period, with other batches soon to

follow. With all the 4137 Co, AM355, and Ardeform 301 U-bends already

under test, only the Vascojet 1000, D6Ac, 300M, and Rocoloy 270

samples remain.

Some difficulty was encountered in springing the higher

strength transverse (primary direction; lowest Y.S.) heat-treated

PH15-7 U-bends into their PVC clips. Fracture of these samples at

the apex of the V (in the cross-section plastically deformed) occurred

upon application of the degree of stress required to attach the clip. It

may be surmised that, for example, the degree of elongation attainable

in the longitudinal (rolling) direction was not sufficient to allow further

deformation. This possibility is indicated by the data shown in Table X

of Report No. 12, containing the heat treatment survey data for this alloy.

LI

£B

8.

The problem was circumvented by placing the V-shaped sample on a

1/2-inch mandrel and then applying sufficient pressure to the sample

ends to allow attachment of the clip.

Rearrangement of the tables of cumulative data has been

undertaken to improve the clarity of comparison of results.

Bent beam specimens of 4137 Co and AM355 are still under

test and U-bend testing of 4137 Co, AMA355, PHI5-7MAo, B12OVCA, and

Ardeform 301 is continuing. A more detailed discussion of the results

to date for these alloys is provided in the following sections of this

report.

Two additional cooperative projects are being undertaken

on the effect of decarburization and alloying on the proneness to stress

corrosion of low alloy missile steels. The information obtained will

be presented at a later date.

a. Bent Beam Tests

The AM355 bent beam specimens (secondary direction)

undergoing stress corrosion testing in the five test solutions (NaCl,

NaSO4 , NaPO3 , NaNO3 and Na 2 S) have produced no failures to date

for any test strength level (7516 of 250, 261, and 302 Kpsi Y.S.), nor

has there been any visual evidence (other than a slight discoloration

in Na 2 S) of any appreciable general corrosion. The cumulative data

for these specimens is given in Table IV.

9.

Bent beam specimens of 4137 Co, exposed to two natural

environments (marine and semi-industrial) by U. S. Steel Applied

Research personnel in a cooperative program, have undergone no

change in status during the report period. The cumulative results to

date are given in Table V.

Similar 4137 Co bent beam samples exposed to an industrial

environment by this Project are reported in Table VI. There have been

a few sample failures during the report period, none of which have

included samples tempered at 1100 0F for any Y. S. test level exposure.

Comparison of the results to date from Tables V and VI (75% of Y.S.

only) reveal the anomaly discussed in previous reports, i.e., the heavy

industrial environment provides less susceptibility to stress corrosion

than the mild industrial or marine environments. This variation from

the expected is not immediately obvious, since sample preparation was

identical, but is thought to be a function of sample preparation after

heat treatment.

Tables V and VI also indicate that an UOOF temper ( 75% of

the maximum attainable Y.S. for this alloy) seems to provide immunity

from stress corrosion, regardless of the test stress level (the tensile

curve for this alloy shows little if any deviation from a straight line

function up to the yield point). Stress corrosion susceptibility of this

alloy may therefore be a function of the Y. S. attained by tempering.

I

10.

Bent beam specimf is for D6Ac, Vascojet 1000, 300M,

P1l-5-7Mo, B1ZOVCA, and the remaining direction of AM355 are

expected to be all under test during the following report period.

b. U-Bend Tests

While all strength levels for the various assigned high strength

steels and alloys and additional, selected alloys are not as yet under

test, the cumulative U-bend test results to date are discussed in the

following sections of this report.

1. AM355 - Only the lowest Y. S., primary direction,

U-bend specimens are not under test for this alloy and, in view of the

results to date, testing of added specimens seems unnecessary. The

cumulative results for the low strength level (250 Kpsi Y.S. in secondary

direction) samples shown in Table VII, the intermediate strength level

(261 Kpsi Y.S. in secondary direction) samples, shown in Table VIII,

and the high strength level (302 Kpsi Y.S. in secondary direction)

samples, shown in Table IX, indicate a possible susceptibility to stress

corrosion in NaCl only. If this were a structural weakness, it would be

one in the direction of rolling (normal to the sample failure, since

failure is predominantly associated with primary or transverse samples).

As Table X indicates, neither AM355 nor PHl5-7Mo seem to

be susceptible to carbon tetrachloride, pentane, or trichloroethane,

although the higher-strength levels of PH-15 are not represented.

S1it.

2. PH15-7Mo - The cumulative results for the low

(201 Kpsi Y. S., primary direction), intermediate (208 Kpsi Y.S.,

primary direction), high (244 Kpsi Y. S., primary direction), and

maximum strength (286 Kpsi Y. S., primary direction) levels, as

presented in Tables XI through XIV, indicate no susceptibility of this

alloy in any of the test environments. However, the higher strength

specimens have not been exposed to testing for too long a period and

any conclusion drawn would be preliminary at best.

3. B12OVCA - The cumulative results for the as.-received

Primary Heat (Table XV) and Comparative Heat (Table XVI) show no

susceptibility of this alloy to stress corrosion in any of the test solutions.

The data, however, are largely inconclusive and the foregoing may be

considered on a provisional basis, since greater bulk of the data are

very short range. The higher strength samples will be in test for

comparison in the next report.

4. 4137 Co - Table XVII data indicate that this low

alloy missile steel is susceptible to stress corrosion failure in all test

environments in widely varying degree. In general, the lower Y.S.

(higher tempering temperature of U000F) samples were shown to be

susceptible only in the phosphate and nitrate environments, the chloride,

sulfate, and sulfide solutions having considerably less effect. The

U-bend test data correlate on a general basis with the bent beam data

I

I

previously given for this alloy in that the percent Y. S. attained with

regard to the Y.S. attainable seems to be one criteria for stress

corrosion susceptibility.

The data in Table XVIII for this same steel show that dry air

and laboratory environments have no apparent effect, whereas those

samples exposed to a moist air environment are prone to failure at the

higher Y.S. levels. Note that the U00*F-tempered specimens are not

affected even in the moist atmosphere.

5. Ardeform. 301 - The cumulative data. for Sample No. I

of this material is presented in Table XIX and for Sample No. 2 in

Table XX. There has been no change in status of these samples over

the last report period. A possible proneness to stress corrosion in the

chloride environment is indicated by the test data.

13.

IV. FUTURE WORK

During the next report period the main research effort will

be directed toward sample preparation, completion of sample heat

treatment, and preparation for presentation of metallographic work.

Cumulative test results on bent beam and U-bend sample

tests for all assigned and additional alloys will be presented.

C. J. Owenrgrr C 'O

W. D. Ruble RESEARCH ASSISTANT

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