21
NRL Memorandum Report 2461 A Procedure for Investigating the Effect of Hydrogen Content on Toughness and Sustained Lead Cracking Resistance of Titanium Alloys, With Some Results for Ti-6AI-4V D. A. MEYN Physical Metallurgy Branch Metallurgy Division June 1972 DDC' R.producud by NATIONAL TECHNICAL INFORMATION SERVICE U S Dlpodrment of Commerce Sprmfield VA 22151 NAVAL RESEARCH LABORATORY Wuhhtc.,D.C. Approved for public release; dianUbution unlingted. ""--,--

A Procedure for Investigating the Effect of Hydrogen

  • Upload
    others

  • View
    2

  • Download
    0

Embed Size (px)

Citation preview

Page 1: A Procedure for Investigating the Effect of Hydrogen

NRL Memorandum Report 2461

A Procedure for Investigating the Effectof Hydrogen Content on Toughness and Sustained

Lead Cracking Resistance of Titanium Alloys,With Some Results for Ti-6AI-4V

D. A. MEYN

Physical Metallurgy BranchMetallurgy Division

June 1972

DDC'

R.producud by

NATIONAL TECHNICALINFORMATION SERVICE

U S Dlpodrment of CommerceSprmfield VA 22151

NAVAL RESEARCH LABORATORYWuhhtc.,D.C.

Approved for public release; dianUbution unlingted.

""--,--

Page 2: A Procedure for Investigating the Effect of Hydrogen

UNCLASSIFIEDSt curmtS Classification

DOCUMENT CONTROL DATA - R & DSecuriII classification of title, body of sbstraert ond mnde~,,ng onnoteor,•ni •root be enered when (fle overall report is classified)

I ONIGINATING ACTIVITY W(orporate author) i2a. REPORT SECURITY CLASSIFICA ION

Naval Research Laboratory UnclassifiedWashington, D.C. 20390 2b. GROUP

3REPORT TiTL.E

A PROCEDURE FOR INVESTIGATING THE EFFECT OF HYDROGEN CONTENT ONTOUGHNESS AND SUSTAINED LOAD CRACKING RESISTANCE OF TITANIUM ALLOYS,WITH SOME RESULTS FOR Ti-6A1-4V

4 OESCRIPTIVE NOTES(T)'pe oireport andinciu•sve dates) T1IiS report completes one pnase of tnetask; work is continuing on other phases.5 Au TPOR4SI (First nfame, middle init•al, last nonme)

Dale A. Meyn

0 REPORT DATE ?a. TOTAL NO OF PAGES 17b. NO OF R!.FS

June 1972 20 1604. CON TRAC OR GRANT NO 9'% ORIGINATOR'S REPORT NuMBERIS)

NRL Prob MO1-08b. PROrC T NO NRL Memorandum Report 2461

Task WR 022-01-01C. ,', OTHER REPORT NO(S) (Arn) other numbers that may be assigned

this report)

IC 0IST RiI8 ION STATEMENT

Approved for public release; distribution unlimited.

. SSPPLEMENTARY NOTES I SPONSORING N'IL'TARY ACTIVIT-

Naval Air Systems Command (52031)Washington, D.C. 20360

.J ABSTRACT

-- A procedure for measuring the effect of hydrogen content on the tough-ness and resistance to sustained load crack (SLC) growth of titaniumalloys is presented. The results of such measurements on a high oxygencontent, very high yield strength heat of 1-in. thick Ti-6AI-4V alloy(R-23B) are compared with results for a low oxygen content, moderatelyhigh yield strength heat (R-14). Both fracture toughness and fLCresistance of R-23B are greatly reduced by small amounts (35 ppm) ofhydrogen added to vacuum annealed specimens. The fracture toughness,but not SLC resistance, of R-14 was likewise affected, in the hydrogencontent range from 9 ppm to 125 ppm.

The present recommended hydrogen content limits of 125 ppm may preventextreme embrittlement in the absence of cracks, but are of no value inreducing sensitivity to SLC. Contents below 35 ppm appear necessary todo that.

The substantial gain in toughness due to vacuum annealing a commercialheat of Ti-6AI-4V (R-23B), without reduction in hardness, raises thepossibility of developing a vacuum annealing schedule for greatly in-creasing the reliability of critical high strength structural parts.

E I

DD, NOV 6,1473 UNCLASSIFIED3/14 0102-014.6600 Securitv Classification

Page 3: A Procedure for Investigating the Effect of Hydrogen

UNCLASSIFIED

-Security ClassificationLIK LNKLN C

SKELIN A LINK 8I C

ROLE WT ROLE WT ROLE WT

Fracture

Titanium alloys

Hydrogen embrittlement

IA

FORM (A~ BACK) UCASFE

II

DDGoE.,,- .-ec.t UNCLASSIFIED(P AGE 21

Security Classification

Page 4: A Procedure for Investigating the Effect of Hydrogen

Contents

Abstract ° ... o... .. i

Problem Status ............. iAuthorization ............. ii

INTRODUCTION ................... ° ......... .. 1

PROCEDURE ........ ... ... ...

EXAMPLES OF RESULTS OBTAINED ................ 5

MISCELLANEOUS RESULTS 6......................6

DISCUSSION ... ....... o ................... .** 7ACKNOWLEDGMENT ....... .... . .... ...... . ..... 8

=.~

.ii

Page 5: A Procedure for Investigating the Effect of Hydrogen

Abstract

A procedure for measuring the effect of hydrogen content onthe toughness and resistance to sustained load crack (SLC)growth of titanium alloys is presented. The results ofsuch measurements on a high oxygen content, very high yieldstrength heat of 1-in. thick Ti-6A1-4V alloy (R-23B) arecompared with results for a low oxygen content, moderatelyhigh yield strength heat (R-14). Both fracture toughnessand SLC resistance of R-23B are greatly reduced by small

amounts (35 ppm) of hydrogen added to vacuum arnealcdspecimens. The fracture toughness, but not SLC resistance,of R-14 was likewise affected, in the hydrogen content rangefrom 9 ppm to 125 ppm.

The present recommended hydrogen content limits of 125 ppmmay prevent extreme embrittlement in the absence of cracks,but are of no value in reducing sensitivity to SLC. Con-tents below 35 ppm appear necessar', to do that.

The substantial gain in toughness due to vacuum annealinga commercial heat of Ti-6A1-4V (R-23B), without reductionin hardness, raises the possibility of developing a vacuumannealing schedule for greatly increasing the reliability ofcritical high strength structural parts.

Status

This report completes one phase of the task; work is con-tinuing on other phases.

Authorization

NRL Problem No. 63M01-08Task No. WR 022-01-01

Page 6: A Procedure for Investigating the Effect of Hydrogen

INTRODUCTION

Titanium alloys are susceptible to sustained load cracking(SLC) due to residual hydrogen at hydrogen contents wellbelow 100 ppm by weight. Experimentation at the NavalResearch Laboratory has established that this crackingoccurs at threshold stress intensity values, KIH, well be-low the corresponding stress intensity for fast rising loadfracture, KIx (or KIc, where this can be properly measured)(1-9). Because these SLC threshold measurements are similarin ambient air (70% relative humidity) (2) and high vacuumenvironments (7,9) for an alloy (Ti-8AI-lMo-IV) which isextremely susceptible to stress corrosion cracking (SCC),it was concluded that SCC was not involved and that alltitanium alloy SLC phenomena in air of ordinary humidityare caused by residual hydrogen.

From this background a useful method has been developed forevaluating the effect of hydrogen content on SLC propertiesin structural titanium alloys. The method utilizes theconcepts of fracture mechanics (10), since effects onmechanical properties of hydrogen contents below 100 ppmare not evident unless precracked specimens are used. Thehydrogen content of the specimens was controlled by vacuumannealing, followed by reannealing in hydrogen to achievethe desired hydrogen contents. Such stringent control isnot required for practical evaluation of the effect ofvacuum annealing on 3LC for specific alloys or lots of onealloy, where reclamation of such material is all that isdesired. Therefore, two procedures will be discussed, oneI dealing with reclamation of SLC-prone alloy lots, the otherwith the determination of specification limits for hydrogencontents in classes of alloys and types of applications.

PROCEDURE

Mechanics

For measuring the fracture toughness KIxor KIc, and thresholdstress intensity, KIH, for SLC of precracked specimens in

- air at room temperatures, the ASTM three-point bend specimenfor fracture toughness measurement (11) is recommended asthe simplest and most convenient to use. If it is desiredto load the specimens as cantilever bars, the stress intensitycalibration of Kies et al. (12) is appropriate in place ofthe ASTM three-point calibration. A bend specimenproportioned according to ASTM recommendations for 1-in.thick material is shown in Fig. 1. The specimens shouldbe of sufficient size and of high enough yield strength sothat the following criteria are met or exceeded (see Fig. 1):

•Z1

Page 7: A Procedure for Investigating the Effect of Hydrogen

S/~KI 2

B 2.5 G'Iys

W-a • 2.5 (K;_-)ys

a a 2.5 'ys

If these criteria are met, values of stress intensity willhave been measured under plane strain conditions, and therecommendations for plane strain fracture toughnessmeasurements (11) can be followed, so that KIc can bemeasured. KIc and KIH can be used tu calculate designcriteria, such as critical crack sizes for fast fracture orsustained crack growth at design stresses. However, avalid determination of KIc is seldom possible for toughmaterials with moderate yield strengths. Hence, it isoften necessary to be content with comparative measurementsof KIx and KIH for nonplane strain conditions, usingstandardized specimens with similar crack lengths. KIx iscalculated using maximum load at fracture and the fatigueprecrack size. Assuming B (Fig. 1) is fixed by platethickness, W should be as great as possible but at leastequal to 2B, S - 4W, and a = W/2.

Side grooves (shallow notches on each side parallel to thecrack) are optional, but if used must be standardizedthroughout the test program. Side grooving will usuallyreduce K values, but may or may not affect KIH measurements.Sandoz M found that for some samples of Ti-8AI-IMo-IV10-20% side grooving halved the thickness necessary to getminimum values of KIH when there was a definite trend ofdecreasing KIH with increasing thickness.

K is estimated by first loading a specimen to about13 KIx, waiting several hours, and then, if no crack growthindications are noted, increasing the load in 10 ksi/:-n-.increments, allowing each load to remain several hours.Some indicator of crack movement such as a deflectionindicator or the ASTM crack opening displacement (clip) gage(11) should be monitored so that one can tell whether thecrack is propagating, or whether the load should be increasedat the end of some time interval. The lowest initial valueof KI resulting in sustained crack propagation and eventualfracture, based on the average crack length measured on thefracture surface (11), is recorded with the total time at

2

Page 8: A Procedure for Investigating the Effect of Hydrogen

the !,ad. This step loading procedure will provide accurateestimates of KIH for specimens with ordinary commercialhydrogen contents, provided the specimen is never unloadedand reloaded. Two other specimens should be loaded to valuesof KI which are 5 or 10 ksi/lii. below and above this value,and the times to failure (or to "run-out" if no failureoccurs) recorded. In addition, times to failure for stressintensity values between KIH and Kix are useful forestimating crack growth rates. This series of measurementsis repeated for each hydrogen level to be investigated.

Thermometallurgy

A. Vacuum Dehydrogenation--The simplest procedure for

determining the degree of vacuum annealing necessary toraise KIH and KIc to some desired minimum value is to try aseries of time-temperature schedules in the actual productionvacuum furnace, or in an accurate laboratory prototype, andtest as outlined above. If the specimens are to be heattreated after vacuum annealing, such heat treatment canbe done in air, since the oxide layer which forms in airwill prevent hydrogen from entering or leaving the specimenexcept possibly at very high temperatures and long exposuretimes. Generally, the highest temperature which will notmetallurgically degrade the material, a good vacuum, andlong times are needed to confer the greatest benefits.Ordinary vacuum facilities with ultimate pressures greaterthan 1 micron (10-3 mm Hg) are not suitable for the purpose,since the equilibrium hydrogen pressure exerted by a typicala-3 titanium alloy containing 20 ppm hydrogen by weight, at16000 F, is less than 1 micron (14). Consequently, thepartial pressure of hydrogen from all sources in the systemmust be kept well below 1 micron to extract hydrogen fromthe alloy, because a hydrogen content of 20 ppm may well betoo high (KIH too low) for critical applications in somealloys. Since pressure readings are ordinarily made atsome point remote from the specimen using gages calibratedfor nitrogen, very low indicated pressures may be needed toattain acceptably low hydrogen contents after annealing.For example, specimens of Ti-6A1-4V held at 17000 F for7 hours at an indicated total pressure of 2 x 10-6 mm Hgstill retained 9 ppm of hydrogen. Tables in Reference 14indicate that such a pressure at that temperature shouldhave reduced the hydrogen content to less than 1 ppm within2 hours. It has been found that the lowest hydrogen contentsin that particular furnace are obtained by annealing at13500 F for 40 hours, a time dictated more by the outgassingcharacteristics of the total system than by the time requiredfor effusion of hydrogen from the alloy. A thorough studyof Reference 14 is recommended before a vacuum degassingschedule is decided upon.

3

Page 9: A Procedure for Investigating the Effect of Hydrogen

B. Method for Varyino Hydrogen Content--The followingprocedure is suitabls for varying the hydrogen content oftitanium alloys in - !.r to quantitatively evaluate theeffect of hydrogen r. tent on the fast rising load (Kix)and sustained load (KIH) cracking resistance of titaniumalloys. The initial step is to essentially dehydrogenateall specimens by vacuum annealing. Kix and KIH measurementscan 'hen be made on the vacuum annealed spec.mens and onrehyd7ogenated specimens.

An ar.t -atu-; for precision re-hydrogenation is shown inFig. The ,a"_uum annealed snecimen is placed in thequar.. "ube, whj',, is then eva:ýuated and heated to 17000 Funder .uui,. V,-e. 17000 F is reached, hydrogen is admitted,all va:,es e .;I . except No. 2, and the requiredpressuie of hyr!- - is bled i-Zo the calibrated volume viavalve 3. The ,aure is computed from the specimen mass(W, grars), the required hydrogen concentration (C, ppm),and the calibrated volume (V, cubI: centimeters) from thefollowing ^ormula:

P (mm Hg)=9.3W

After the proper pressure is attained, valves 2 and 3 areclosed, valve 1 is opened (4 remains closed), and thesystem (except the calibrated volume) is reevacuated.Valve 4 is then opened, all other valves are closed, andvalve 2 is opened to admit hydrogen to the specimen. Afterthe 0-760 mm gage reads essentially zero (a few minutes),valve 4 is cl-sed. The system remains in this conditionfor 7 hours to ensure homogeneous distribution of thehydrogen in the specimen. The furnace is then allowed tocool to a temnperature at which the specimen can beconveniently removed, or the quartz tube can be extractedfrom the furnace for faster cooling. 17000 F for 7 hourbwas selected as a condition which was fairly certain togive a complete absorption and uniform listribution ofhydrogen in a 1-in. thick specimen. Experience indicatesthat a lower temperature, e.g., 15000 F, could be expectedto give equally good results. The following points must beconsidered in selecting a treatment cycle: 1) Surfaceoxides must be completely dissolved, hence temperatures be-low 13000 F, at least for initial absorption, are risky.2) The diffusion rate of hydrogen in titanium (which isdifferent for a and B phases), is temperature dependent(14), For example, 7 hours at 17000 F is roughly equivalentto 30 hours at 13500 F, for absorption and homogenization.3) The initial absorption time is not thickness dependent,but the achievement of a uniform hydrogen distributiondepends on diffusion, and diffusion times are roughly pro-portional to the square of the thickness for a given temperature.

4

Page 10: A Procedure for Investigating the Effect of Hydrogen

EXAMPLES OF RESULTS OBTAINED

Ter" have been conducted on two heats of Ti-6A1-4V (Table 1),one containing 0.19% oxygen (R-238), the other containing I

t" 0.07% oxygen (R-14), to show how hydrogen affects thesustained load (KIHY and rapid rising load (Kix) crackpropagation resistance of a typical high strength titaniumalloy. The results are tabulate. in Tables 2 and 3.Figure 3 summarizes the efect of hydrogen content on KIxand KIH. All measurements were made on transverse (WR)specimens.

R-23B (0.19% oxygen) 145 ksi yield

Because the hardness of R-23B specimens was not reduced byany of the annealing treatments, and because the measuredyield strength did not decrease after annealing in air at17000 F for 7 hours and furnace cooling, it is believedthat the yield strengths for all the conditions reportedhere were essentially the same.

The low toughness and SLC resistance of the as-receivedplate was substantially raised by simple annealing in airat 17000 F for 7 hours and furnace cooling. This toughnessand SLC resistance were further increased by annealing theas-received material in a vacuum (5 x 10-6 mm Hg) at 17000 Ffor 7 hours and furnace cooling. Except for these effects,changes in hydrogen content over a wide range above 35-50ppm had little effect on KIH or Kix. The principal effectof increasing hydrogen contents above 34 ppm is to increasethe sustained load crack growth rates, as indicated by thegreatly reduced failure times near KIH for specimens withhigher hydrogen contents.

The reports in earlier work (13) that Ti-6AI-4V does notsuffer embrittlement at hydrogen contents below 400 ppmwere based on smooth or notched tensile specimens, whichobviously are unsuitable for evaluating the effect ofhydrogen content on toughness.

The few approximate values of Kic in Table 2 (specimens 289,290, and 267) are for as-received and air annealed specimens.For these, KIH is about 75% of KIc. This ratio is represen-tative for as-received Ti-6A1-4V alloys which have been testedat NRL.

The specimens containing 122 ppm of hydrogen behavederratically, possibly because they are sensitive to steploading (increasing the load after long intervals at previousloads). However, one specimen failed at a fairly low value

5

Page 11: A Procedure for Investigating the Effect of Hydrogen

of KI (No. 280) in spite of step loading, while the othersdid not fail until much higher KI values had been imposed.There were no irregularities in the fatigue-precrackprocedures or crack front shapes, nor was anything sur-prising discovered on the fracture surfaces, which waresimilar to those of all the other "KIH" specimens. Al-though such behavior makes estimation of KH difficult,it is reasonable to place KIH at 58 ks iTn., where No. 280failed, since this continues the trend established by theother hydrogen contents.

R-14 0.07% oxygen, 124 ksi yield strength as-received

The fast fracture toughness index, Kix, for R-14 decreaseswith increasing hydrogen content in the same way as forR-23B, but KIH is not obviously affected. Although thespecimens are under-sized with respect to the plane straincriteria mentioned earlier, it is hard to blame this factorfor the lack of KIH variation with hydrogen content, sinceKix definitely increases with reductions in hydrogen in thesame size specimens. Further reduction of hydrogen below9 ppm might raise KIH, because such a reduction (to 5 ppm)did have this effect on R-23B. ýThat is, 9 ppm may besufficient to fully "embrittle" R-14 with respect tosustained load cracking. The as-received toughness and SLCresistance of 1-in. thick specimens of WR orientation canonly be inferred from measurements on 3/4-in. thick WTspecimens by Beachem, et al. (15). Those results wereconsistent with those obtained on the air annealed RWspecimens tested here. In contrast to its effect on R-23B,

high hydrogen contents do not markedly increase crack growthrates in R-14. This, again, may be attributed to the lackof hydrostatic constraint (plane strain) afforded by thelow yield strength at this thickness.

MISCELLANEOUS RESULTS

Annealing in air for 1 hour at 1700' F did not significantlyraise the hydrogen content of vacuum annealed specimens ofR-23B (Table 2, No. 294 and No. 295), and the hydrogen contentof R-14 after annealing in air for 7 hours ac 17000 F was38 ppm, which is about equal to the producer's analysis(Table 1). On the other hand, the measured hydrogen contentof R-23B specimens after annealing in air 7 hours at 17000 Fwas 65 ppm, compared with a measured 34 ppm in an as-receivedspecimen. It is difficult to decide whethe: to blamevariations in hydrogen content in the plate, or to concludethat prolonged annealing at high temperature in air increasedthe hydrogen content in R-23B, but not in R-14.

6

Page 12: A Procedure for Investigating the Effect of Hydrogen

The chosen temperature, 17000 F, and annealing time, 7 hours,provided a completely uniform hydrogen distribution in allthe specimens. Analyses for several locations from the sur-face to the center showed no consistent variations in hydro-gen content within a given specimen. The absence of ahydrogen content gradient in vacuum annealed specimens sig-nifies that the ultimate vacuum attained in the furnacedictated the hydrogen content of the specimens, and thathydrogen contents well below 8 ppm could be attained within7 hours at 17000 F if the partial pressure of hydrogen at thespecimens surface could be reduced.

DISCUSSION

The data presented here are based on 1-in. thick specimens, Iwhich are not large enough to satisfy the plane straincriteria presented in the beginning of this paper for R-14,but are satisfactory for all but vacuum annealed R-23Bspecimens. Although the numerical values of fracturetoughness are not all useful for design purposes, the trends

observed are useful and surprising, and point to some prom-ising directions for titanium alloy metallhrgical research.The "inevitable" embrittlement of Ti-6AI-4V by the additionof oxygen to raise the yield strength seems to somehow betied to the presence of hydrogen. While KIH of R-23B in-creasc with a decrease in hydrogen content as expected, thetoughness increased at least as much, without any observabledecrease in hardness, and thus strength. The substantialincrease in KIx and KIH due to annealing at 17000 F in air,and the further increase in Kix and KIH due to annealing invac'uum, without loss in hardness compared with the as-

received plate, leads to two conclusions. Ff.-st, commercialTi-6A1-4V plate does not receive heat treatment calculatedto optimize its toughness at high yield strength. Second,the combination of an optimum heat treatment with vacuum-dehydrogenation promises to yield a very high toughnesswhile retaining high yield strengths.

The comparison between R-14 and R-23B is somewhat complicatedby their differences in yield strength, but the superiorityof the low oxygen content alloy is only apparent in thesetests as a higher KIH at moderate and high hydrogen contents.When both are vacuum annealed, their KIH values are identical.The most important observation, however, is that both aremuch tougher after thorough dehydrogenation.

Although KIH does not decrease with continued increase inhydrogen content above 35 ppm (in R-23B), the rate of crack-ing, reflected by time to failure above KIH, does increase.

7

Page 13: A Procedure for Investigating the Effect of Hydrogen

R 7V-j - 'W

For example, the failure times of specimens with 206 ppmhydrogen change front hours to minutes over a span of 4ksifin., near KIH. SLC evidently is a stress dependentprocess, whose rate is controlled by the rate at which acritical local hydrogen concentration can be attainedthrough diffusion to the region near the ciack tip. It ispossible that KIH increases (in an operational sense) atvery low hydrogen content because some competing process,such as creep-induced stress relaxation, forestalls cracking.

The present recommended limit for hydrogen in titaniumalloys is 125 ppm. This limit is based on experience withplain or notched, but rot cracked, tensile specimens, andevidently is of little value in controlling the sensitivityto SLC of titanium alloys. It serves mostly to preventreally appalling embrittlement problems from occurring. IfSLC is to be eliminated, either hydrogen contents must bekept below 10 ppm, or some other approach to preventingSLC must be found.

The complex effect of hydrogen content on the toughness ofR-23B cannot be explained with existing knowledge oftitanium alloy metallurgy. In order to fully exploit thepotential for good combinations of strength and toughnesswhich may be attainable by as yet unthought-of changes inalloy chemistry, and thermomechanical processing, a morecomplete understanding of the possibly synergistic effectsof interstitial and substitutional alloy elements and ofprocessing techniques is necessary. In the context of thepresent results, the metallographic strengthening mechanismof oxygen, and the influence thereon of hydrogen, zindpossibly of other components, is a mystery which has neverbeen truly explored, the understanding of which might makepossible new trends in engineering alloy development.

ACKNOWLEDGMENT

This research was supported by the Naval Air Systems Command.

!B

Page 14: A Procedure for Investigating the Effect of Hydrogen

REFERENCES

1. G. Sandoz and R.L. Newbegin, "Delayed FractureCharacteristics of Ti-8A1-lMo-IV Alloy," Report of NRLProgress, May 1967, pp. 31-32.

2. G. Sandoz and R.L. Newbegin, "Effect of Hydrogen Content

on Subcritical Crack Growth in Ti-8A1-lMo-lV Alloy,"Report of NRL Progress, Nov 1967, pp. 35-36.

3. G. Sandoz and R.L. Newbegin, "Effects of Hydrogen Contenton Subcritical Crack Growth in Two Ti-8A1-lMo-IV Alloys,"Report of NRL Progress, May 1968, pp. 31-32.

4. G. Sandoz and R.L. Newbegin, "Effects of Hydrogen Contentand Environment on Subcritical Crack Growth in Ti-7A1-2Cb-lTa and Ti-6A1-4V Alloys," Report of NRL Progress,Nov 1968, pp. 31-32.

5. G. Sandoz, "Subcritical Crack Propagation in Ti-8AI-lMo-IV Alloy in Organic Environments, Salt Water, and InertEnvironments," Proceedings of Conference: FundamentalAspects of Stress Corrosion Cracking, Ed. by R.W. Staehle,A.J. Forty and D.van Rooyen, NACE (1969) pp. 684-69").

6. D.A. Meyn, "Cleavage Cracking of Ti-8A1-lMo-lV UnderSustained Load in a Vacuum and in Methanol," Sept 1969,pp. 34-36.

7. D.A. Meyn, "Effect of Hydrogen Content on SustainedLoad Cracking of Ti-8AI-lMo-IV in Vacuum," Report ofNRL Progress, Sept 1970, pp. 30-32.

8. D.A. Meyn, "Hydrogen-Assisted Cracking in High StrengthTi-6AI-4V Alloy," Report of NRL Progress, Mar 1971,pp. 16-18.

9. D.A. Meyn, "Effect of Hydrogen Content on Hydrogen-Induced Cracking of Ti-8AI-lMo-lV," Report of NRLProgress, Dec 1971, pp. 11-12.

10. B.F. Brown, "The Application of Fracture Mechanics toStress-Corrosion Cracking," Metallurgical Reviews,Vol. 13 (1968) p. 171-183.

11. "Tentative Method of Test for Plane-Strain FractureToughness of Metallic Materials," 1970 Book of ASTMStandards, Part 31, p. 919.

9

Page 15: A Procedure for Investigating the Effect of Hydrogen

12. J.A. Kies, H.L. Smith, H.E. Romine, and H. Bernstein,"Fracture Testing of Weldments," ASTM Special TechnicalPublication 381 (1965) p. 328.

13. R.I. Jaffee and D.N. Williams, "The Effect of Composi-tion on the Hydrogen Embrittlement of Alpha-BetaTitanium Alloys," Trans. ASM, Vol. 51 (1959) p. 820.

14. W.M. Albrecht and M.W. Mallett, "Hydrogen Solubilityand Removal for Titanium and Titanium Alloys," Trans.Met. Soc. AIME, Vol. 212 (1958) p. 204.

15. R.J. Wasilewski and G.L. Kehl, "Diffusion of Hydrogen

in Titanium," Metallurgia, Vol. 50 (1954) pp. 225-230.

16. C.D. Beachem and D.A. Meyn, "The Effect of Thicknessupon Sustained Load Crack Propagation in Ti-6A1-4VTested in 3j% NaCl Solution," NRL Report (to bepublished).

10

Page 16: A Procedure for Investigating the Effect of Hydrogen

Ca9

w 0 00

H -4

00 c 0CH r f

co 0 - ; 400

C400 0

CDd

00

E-el00

00

00

0 -4

LU0 *0q -

0~ ~ 0EM1

03 00 C

H4 C'I 4 LU

Page 17: A Procedure for Investigating the Effect of Hydrogen

Table 2 - R-23B (0.18% oxygen) Experimental Results

First Load Final LoadHard- Est. (no cracking) (cracking)ness Hydrogen Y.S. XI Time Ki Time

I.D. No. Thermal Treatment* (Rd) (ppm) (ksi) (ksai/Tr.) (hr) (ks i/Tn) (hr) Comments

289 as-received 34.5 34 145 - 58 0 KIx-(Klc 511290 ns-received 34t 145 - 63 0 K .(K T54292 as-received - 34t 145 - - 40 20.1 chtil9er303 as-received 34t 145 - - 42 10.7 cantilever

266 1700Air7FC - 65 145$ - - 86 0 Kyx267 1700Air7FC 34.0 61 145 - - 87 0 Klx.(Kjc ý 77)273 1700Air7FC - 65t 145 - - 63 2.1 cantilever281 1700Air7FC - 65' 145 - - 70 0.5 cantilever282 1700Air7FC - 65 145 - - 60 3.3 cantilever

297 l70OArgonTFC - 34t 145 - - 72 0 Kix305 170OArgon7FC - 34' 145 - - 103 0 Kix258 1700Argon7FC - 34t 145 - - 60 8.9 3-point296 1700Argon7FC - 34t 145 - - 70 0.0005 cantilever306 1700Argcn7FC - 34t 145 51 25.9 61.5 19.1 cantilever

261 1700V7FC 34.0 8 145 - - 132 0 Klx265 1700V7FC - 8t 145 - - 132 0 KIx270 l700V7FC - 8+ 145 - - 129 0 KIx257 1700V7FC 34.0 7 145 - - 84 8.0 3-point262 1700V7FC - 8t 145 - - 84 15.2 3-point263 1700V7FC - St 145 - - 103 2.3 3-point264 1700V7FC - St 145 - - 92 6.7 3-point

268 1700V7FC+1350V40FC - 4.5t 145 - - 129 04Q9 1700Y7FC+1355040FC 34.0 4.5 145 72 6.4 99 56.4 3-pxoint

295 170OV9OFC+I70OAlAC - lit 145 - - 124 - Klx294 I?OOV9OFC+1700A1AC 33.0 11 145 83 20.9 94 15.0 3-point

304 1700V7FC+1700H27FC - 36t 145 - - 105 0 Kix291 1700V7FC+1700H2 7FC - 36 145 - - 110 - Kjx293 1700V7FC+1700H27FC 34 36 145 - - 59 19.8 cantilever

'775 1700V7FC+1700H27FC 34.5 53 145 - - 95 0 KIx288 170OV7FC+1700H27FC 34 47 145 - - 95 0 KIx276 1700VTFC+1700H27FC 35 50t 145 - - 61 6.1 3-point302 1700V7FC+1700H2 7FC - 50t 145 62 95.6 66 4.2 cantilever

279 1700V7FC+1700H2 7FC - 122 145 - 91 0 Kix310 1700V7FC÷1700H2 7FC - 122t 145 - - 89 0 Kix2h0 1700V7FC+1700H27FC 34 122t 145 47 1.25 58 0.2 3-point286 1700V7FC+1700H27FC 35 122t 145 53 4.2 75 0.12 3-point301 1700V7FC+1700H 2 7FC - 122' 145 60 21.5 81 0.033 cantilever309 1700V7FC+170OH 2 7FC - 122T 145 63 2.1 70 5.3 cantilever

307 1700V7FC+1700H 2 7FC - 206t 145 - - 91 0 KIx318 1700V7FC+1700H 2 7FC - 206' 145 - - 83 0 Kix314 1700V7FC+1700H2 7FC 34 2060 145 - - 64 0.17 cantilever315 1700V7TC+170OH 2 7FC - 2061 145 - - 64 0.13 cantilever316 1700V7FC+1700H2 7FC - 206t 145 - - 62 2.7 cantilever317 1700V7FC+170OH 2 7FC - 206t 145 - - 60 4.3 cantilever

0 1700V7FC - Annealed at 1700' F in vacuum for 7 hours, then furnace cooled, for example.

t Estimated hydrogen content. No analysis available.

Measured transverse 0.2% offset Y.S.

All Kix and Kic measurements 3-point bend. Maximum load reached in 10-15 seconds, crosshead speed 0.005 inches/second.

12

Soi

Page 18: A Procedure for Investigating the Effect of Hydrogen

r-4~ lz9: t;

C) .4.. 4 ..4 -1 -H 4-)42 4444 0 44 00 .4

0 142At 1.40 H 1 IS14 14 1400 0

*~ P)

o iz -4 H~f r4 H 0 (AC

H.NO H H CU HOI4

0~ a~H

4-i- ~ ~ ~ c 4- 4 -- --- C

CD 0 0

o4 U Ar2 ot

64. 01 0 U.. Cd' 0 0 00 0 0 1 02

4) $4 0

-q 2C - tI- 0to 0 r-4 C)

CUC) be a) 4- 4- C0 00i OD Or, (7) zD M 0 V 0 -

$44 Cf) CV )m 000

0.0I0

H o o0 0 00 000 0 >)

P4 M ~ . - 2 - - H C-)rIr-

H .,44 0 00 000 CU 0) 0)c

4) 000 OD 0 00 000 C: ..2I 000 0000 0

IH r4 44* IC t' C

- ~:HI'C ~0o, C~CC0)

Page 19: A Procedure for Investigating the Effect of Hydrogen

~ ~ ; ~ ~ -7h

I

I£I2

IIg I

*_ "

144

Page 20: A Procedure for Investigating the Effect of Hydrogen

cr.

4W _ ___

_~j ML

=0 -L

wI 0

Nj wir . ar

4n 9)wmoo

w0Nw

CDwWW E o

I-It 0N

co

CL)

ow Ww CodI

0; I

Ir-LD34-j Cf

0 Cf) w CL Ccn W Q) 15

M cr I-> 0 4

Page 21: A Procedure for Investigating the Effect of Hydrogen

ISO -EFFECT OF HYDROGEN CONTENT ON TOUGHNESS AND S.L.C.

Ti-6AI-4V (R238) I INCH PLATE

160 Y.S.- 145 KSI TRANSVERSE0.18% OXYGENA&1 VACUUM ANNEALED 8 HYDROGENATED 34.5 Rez 140 - 0O AS RECEIVED 34.5"Rc

A ED ANNEALED IN AIR , 1700F 7 HOURS 34.5 Rc

Z \A, I" PLANE STRAIN LIMIT

60 "- -' -------------- A.-',-

20--

(j)80 "XKII

20 60 6I-A-0 816 A0)

40- 0

20

0 I I I I I I I I I I IO 20 40 60 80 I00 120 140 160 180 200 220

HYDROGEN CONTENT, PPM

(a) - R-23B

180-- EFFECT OF HYDROGEN CONTENT ON TOUGHNESS & S.L.C.Ti-6AI-4V(RI4) I INCH CUT FROM 3 INCH PLATE

160 Y.S.v 110-115 KSI TRANSVERSE0.07% OXYGENAA VACUUM ANNEALED B HYDROGENATED 28-30 Rc

140 -D ANNEALED IN AIR 01700OF 7 HOURS 30Rc

120 -AKX

z KIH A

u80) A A AU) 0 I" PLANE STRAIN LIMIT- 60-

u)

40

20

c 1 I I I I I I .I I I i0 20 40 60 80 100 120 140 160 180 200 220

HYDROGEN CONTENT, PPM

(b) - R-14

Fig. 3 - Effect of Hydrogen content on Kjx and KIH.

16