UNCLASSIFIED / LEHAFFED ss as16149 uniimited TA Four 4 roo 010 BL ELIE Research and Development on Titanium Alloys BATTELLE MEMORIAL INST COLUMBUS OH 31 OCT 1949 Distribution authorized to DoD only; Administrative/Operational Use; 31 OCT 1949. Other requests shall be referred to Air Force Materiel Command, Wright-Patterson AFB, OH 45433-6503. Pre-dates formal DoD distribution statements. Treat as DoD only. unlimited ZAW UNCLASSIFIED / H1M4EFED we oro g2FUNCLASSIFIED / EHMHFED— Redistribution Of DTIC-Supplied information Notice All information received from DTIC, not clearly marked "for public release” may be used only to bid on or to perform work under a U.S. Government contract or grant for purposes specifically authorized by the U.S. Government agency that is sponsoring access OR by U.S. Government employees in the performance of their duties. 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(Game) for AMC, Wright-Patterson Air Force Base, Dayton, 0. Gers) Unclase, ws Engiish 126 tables, dlagrs, grants (Same) ‘Progress ts reported in develowment of tateatum alloys, Phaxe relations in titaniem - 0 to 1% get: ‘were investigated. Nickel was fom to limit markedly (he jam A meet the teanlle strength asd lowered the Gact¥lity of Process A titantam, Ternary alloys of managese and carbon, mongenece snd vazadius, aif nclybdenear and bengaten, prepared by eAéing ie pare metals jdoring arc metting, had quite erratic tensile properties when tested after fabrication to sheel, Teste / were completed os evaluation cf "hot-pressed" titantum carbide and graphite cractiles, Coptes obtainable from CADO_ . ‘Thtentamn alloys ‘Matertals (8) Wis, Non-Farrocs Metalsand Alloys 12) USAF Contr, No, AF $3(038)-3738BATTELLE MEMORIAL INSTITUTE couvmics 1, oxo Noverter 12, 19h ’ AF 909 $0 “rightFatterson dir Fores Base Service Area ~ Bulléine 255 Dayton, Ohio Attention MOREA - Contract No. AF 33{038)-3736 Gentlenen: Bnelosed are thirty (30) cories and one (1) repreducitle of ‘the Second Progress Report prepared urder Cortract No. AF 33(038)-3736. ‘This report contains an account of the followings 1. A deseription of the alley developnent. wore done during the bincnthly period September 1 to “Gctover ZL, 19h9. 2, The progress made during the sane period an ‘the develepnent of refractories for holding nolten titanium. 3. Further work on the vacuun-fusion technigae for determining oxygen in titanium, Very truly yours, L, % Eastwood ibeSECOND PROORESS REPORT COVERING THE PERICD SEPTQMER 1 7O OCTOBER 3, 19h9 RESEARCH AND DEVELOPMENT ON TITANIUM ALLOYS. Contract Ne. 33(038)-9736 to “RIGET-PATTERSON ATR FORCE BASS DAYTON, OHIO BATTELLE JENGKLAL INSTITUTE Sotcber 32,L9l9 seri a» le ah hie A A A Ro ‘BATTELLE MEMORIAL INSTITUTE,‘TABLE OF Page, TMTRODCTION, 6 ee eee & ARC MELTING SETANIUM-BASE ALLOWS. ee ee ee ee 62 EVALUATION OF EXPERIMENTAL TITANCUM-BASE ALLOWS...» 65 Binary Alloys of Titanium see eee eee eee 6S Titaniumsslver Alloys. sss ee eee 8 Mechanieal Properties, +++ e+e e ees Th Structure and Transformation Ranges + e+ 7h Heat Treatment. oe yee ee eee ee eee Th MtanionBeryiliun Alleyss ee eer ee ee ee Mechanical Fropertie: eee B Structure and Transformation Ranges +e. 6 + 78 Heat Treatnent. oes ee eer ee ee BO ‘taniunZircontum AMOS. ee ee ee ee BO Mechanical Properties. see eee eee + BO Structure and Transformation Ranges oe ees 82 Heat Treatment. os ee ee eee ee ee BR TehentumColumbiun LVS. ee eee OB Mechanica) Fropertiess see eee ee eee BS tamtumtantalin AMS. oe ee ee ee 8S Wiechanical Properties. 6. ee eee ee 8S ‘Dernayy Abloys of Titanium se. eee eee ee 8B Evaluation of the Alloys of Greatest Interest... 92 i BATTELLE MEMORIAL IeETTTUTE,‘TABLE OF oowrams — (CONTINUED) DWESTICATION OF REFRACTORIES FOR NELTING TETANTIM. « «+ AMLYTIOAL MBTHODS FOX TITAMIUWBAST ALLOWS. oe eee Studies on the Chemical Analysis of Oxygen in ‘TAtaniun by the Chlorine-Carbon Tetrachloride Methods eee ee eee ee eee ett et eee ‘The anslysis of Tktaniun fer oxygen by Vaouumefusion Hethods) vee ee ee et eee Freparation of the Standard Samples, es + ee +e ‘The Derge ethod of Analyzing fer Oxygen in Titanium by Vacuun Fusion, wes ee ey Apparatus ant Genera? Techatquesy ys ee es ‘The analysis of Titanium. see ee eee Notes and Comments, s+ eee eee tees ‘The Recults fram Vecuim-Fusion analysis. «+ FUTURE WRKe eee eee ee et eee eee Page, 96 87 +97 105 “105 209 209 ne 13 ay ny i : BATTELLE MEMORIAL HORTUTEPRES err en ‘SBCOND PROGRESS REPORT COFERING THE PERICD SEPTEMUER 1° TO OCTOBER 31, 19h9 on RESEARCH AND DEVELOPMENT ON TITANIUM ALLOYS Contract No. AF 33(038)=3736 te WRIGHT-PATTERSON AIR FORCE Bust ‘DAYTON, OHIO fre BATTELLE MEMORIAL THSTITUTE October 31, 1949 ‘SrROARY ‘The phase relations in titaniun-0 te 1 per cent germaniun and titanium ~ 0 to 10 per cent mickel alleys were investigated, The addition of germaniun to Frocess A metal was found to raise the beta and lower the alphe solvus lines, No germanium-rich phase was observed. Yickol was found to Limit markedly the alpha-phase field and to ower the beta solvas Line. A nickel-rich phase appesred in the micro~ structure of the alloy containing about 7,5 per cent nickel when the specizen was quenched from 150°F. The eutectoid composition in the binary ‘titantumeniekel system is placed between 6 and 7 per cent nickels In the binary titaniun-silver system, the range cf compositions Anvestigated was extended to $.0 per cent silver, and titaniun-berylitun, alloys containing 0.1 to 1.0 per cent beryllium were investigated. Nene of those alloys bad tensile properties of interest. Binary titantumsirconium alloys containing additions of 1 to 10 per cent strconiua were aise studied. ‘Wo alloys of interest were noted. BATHOLE WENA WESTTTUTE, sere cn mananavee 1 : Additions of 1 and 2 per cent columbium or tantalun to Frecess A fetal were found to increase the tensile strength and Lower the ductility lof Process A titanium, ‘The range of these ctloying additions will be ex- tended. Ternary alloys of manganese and carbon, manganese and vanadium, jand molybdenum and tungsten, prepared by adding the pure netals during are melting, were found to have quite erratic tensile properties when tested after fabrication to sheet. This condition is attributed te incomplete melting and nomuniform distribution of the alloying metals during arc melt~ ing. The use of master alloys, or hardeners, for introducing the atloying additions was investigated, This practice appears, in the Linited tests conducted, to give greater hemogeneity in the ingot. This melting technique wit be used more extensively in the future, Stops have deen taken to re-evaluate the more promising high~ strength alloys. This work is directed tomard selecting an alloy composition on which extensive engineering data will be obtained. Limited data indicate that the tensile properties can be reprodused on most of these slley composi- tions. Tests were completed on the evsluation of “hot-pressed titanium carbide and graphite crucibles lined with tantalun carbide and turmeten boride as refractories for nclten titariun. Melts were prepared in erucibles nade of zirconium oxide (stabilized with Cad), caleinm oxide, calcium oxide Jftuxed with 0p, and alurinon oxide. The stabilized zirconia wide crus cible vas the first refractory tested which had areas “not wet by the molten ‘titanium, Therefore, additional nelts in this type of crucible are planned to ovaluate this refractory further, ane of the otter refractory mate— rials tested appear to be useful. ~ BATTELLE MEMORIAL tresrrrUrE amen a SU tn a~ , Standard specimens of iodide titaniun, containing known anounts of oxygen added as Tidz, “were erepared and submitted te Dr, G. Derge, ¢f the Carnegie Institute of Technology, for vacuunfusion analysis, The results reported fron this laboratory indicate that the vacaum-fusion technique, as it presently exists, yields fairly reliable results, Relatively minor Anconsietencies in the analytical results were obtalnea. at the present tine, it Le not Imowm whether thie is inherent in tie analytical tecknigue, or merely reflects’ sLight nonuniformity in the conpositien of the sample ingots. TeTRCEC NON During the bimonthly period covered by this report, Septenver 1 te Cctober 32, 199, the experinentel progran on titaniua has contimed, The phases of the work described in this report are as follows: ene SE ETI? AY NE NNN he Are Uiskting Uitanian-Hase Alloys. 2, Srahuation of Experimental Tianiunfase «LLeyss je Unvestigation of Rafractories Cor uel ting Titanium k. analytics? Wotheds for Titaniumase Alloys. ARO LELTDNG TTPANTIIARASE ALLOS ¢ (0. “. Sinmons and ¢, T, Greenige) Approximately thirty-five O.5-pound ingots were mage and scbatted, ik AS MBN A ena os ae for fabrication during the perice September 1 to October 15, 199, The ine tended compositions of the ingots, on which the testing hae been completed, are Listed urder the section on "Syalvatien of Experimental Ti tanian-Base ALiey: BATTELLE MEMORIAL INSTITUTEone 6 Smee difficulty wae expertenced when high-strength alloys contain ing wongarese wore tested. It vax found that manganese hed not satisfacto Uy gone into solution to produce a honogeneous ingot. Jthoygh manganese ia a relatively low-nelting-point matdrial, ite density 1s suftietent to cause St to eink beloy the surfate of the molten bath where it cannot be subjected to the direct heat of the arc, This necessitates solution of a solid phase in the Liquid bath rather than the mixing of to Vienld phases, To counteract thie nonhonogereity, it wes decided thet the mange rete should be aeied tn the form af a master alloy. & 38 per cent manganese ailoy vas prepared by are uelting electrolylic mangenese and Process A titanium, This alloy vas readily crashed and then sereenod to 20-40 lo-nesh lve and usod in preparing three ingots to avaluste this procedures This tectnigue speared to produce more uniforn ingots, and, subsequently, the following mester alloys wore propare 1. $8 per cont chremiun eutectic alloy (crushed readily). 2. 35 per cont manganese alloy (crushed readily). 3. 3§ per cent Aron a¥Moy (crushed readity). k, 3h per ecnt nickel outectic alloy (crushed readily). 5. 36 per cont vanadion alloy (vory difficult te crush). Since the constitution diagran af the aanpaneso-titanium system was not knoun, several small ingots rere prepared for microscopic exanina~ tion. These ingots contained 35, 10, 50, 60, and 70 par cent manganese, respectively, am alloy containing acout 53 par cent manganese vas solentod a5 having essentially a eutectic structure. BATTELLE MEMORIAL INSTITUTE, 3 iSnail test ingots of venadiun and of iron have alse been prepared for microscopic oxanination, The eutectic compositions in these systens will be selected for the master alloys, and the necessary melting stock will be prepared, ~ : ‘Two 2=pound ingeiu of the 5 per cent chromium, 2 pet eent iron, and 0,25 por cent ci. son alley were preparcé for forging. These ingots were melted in the are furnace, using ture metal additions ami a carbon electrode, The carbon addition was made by incidental pickup from the electrode, A.naster alloy containing about 2.5 per cent nitrogen was propared in the following manner: Titanium poyder about LO to 60 nish was treated in the Sievert's apparatus te produce a nitrogen content of about 2.5 per cent. This material was very thorcughly nixed after reaoval fram the apparatus to eliminate any nomunifermity which might exist. The ponder was then comprossed into bars 1/2 inch wide by 1/l inch thick, which were sintered at 1900'F, for 21/2 hours at -G.1-ndcron pressure. The resultant bars wore cut into pellets shout l-mesh sicc to provide stock for adding to the melts. The pelleting procedure savered # double function, As origi~ sally treated, the titanium power was vory difficult to add to the bathe ‘The sna size and low density of the poricr permitted it to be carried out of the molting chanbor by the hot furnace gases. However, the pellets dropped directly to the bath, where they floated until melted by the direct Ampingenent of ths are, This procedure insured a uniform ingot composition through the mixing of tio liquid phesese ‘BATTELLE MEMORIAL INSTITUTE,‘EVALUATION OF EXPERIMENTAL TyTANIUM-BASE ALLOYS (Co Ma Craighead, F. Fawn, and L, % Eastwood) ‘The alloy ovalustion zork during the present bimonthly pariod has Yeon directed toward tho investigation of: 2, Binary titaniumgernenium alloys, 2. Binary titardumenickel alloy. 3. Binary titaniumsitver alloys. A. Binary titanturcbery2linn alloys. 5. Binary titanium-zirconium alloys. 6 Binary titeniue-colmbiun alloys. 7. Binary titenium-tentalun alloys. 8, Ternary alloys of titanium. 9. Evaluation of selected alicys. Binary Alloys of Titanium Jn the provious bimcnthly repert, data on the mechanics) properties] arf the response to heat treatment and aging of titaniungermanium and ti- ‘teniun-nickel alloys vere Listed in Tables 1 ard 2. The microscopic exanina~ tion of specinons of those alloys, quenched fron temperatures of 1450, 1550, 1600, 1650, 2700, and 1750°F., >as now been completed. Table 16 shows the phase relations observed in the titaniumgermaniun alloys. Thess data are shown graphically in Figure 19. . “ith the addition of germaniua, up to about 2 per cont, no ger= snium-rich phaee vas ovident in the structure of the quonched specimens. However, as indicated in Figure 19, tbe addition cf germanium to Process A ‘2itantum raised the bota and lowered the alpha solvus Lincs, (BATTELLE MEMORIAL INSTITUTE. i i |' L r TABLE 16, FRASIS PRESENT IN BINARY TITANIUILGERUMIIU! ALLOYS AT TEMPHRATUAES INDICATED - FRODESS A METAL BASE ‘sot Hoat eat Heat = Heat = Ment’ Heat Heat Intended Rolled ‘Treated Treated Treated Treated Treated Treated Woe _Gomposition, & 14507 150%. 150%, 1600. 1650%. 1700%. 750%. 80-20 15 - 85 W180 Unelleyed «= e . a+B atp B 6 85-15 &-40 5-9 HELO Oe Ge a . a+Bp a+, o+8 B 8 9-5 7-30 10-90 WG? 5 Ge a e a+B a+p e+f 8B 8 90~10 70-30 30-70 WMS 1.0 Ge « * o+B atf a+8B @ 3B eece ce 67 , Ts —— ALPHA PHASE | ALPHA + BETA BETA PHASE 1 | 125 a ? i 1700 165 1600} TEMPERATURE, °F. 1550} I500,--~- 1450-—p: Oo Ol 02 03 04 O5 O06 OF AB O9 10 GERMANIUM, PER CENT FIGURE 19. TENTATIVE DIAGRAM SHOWING TRANSFORM- ATION RANGE OF TITANIUM-O TO 1.0 PER CENT GERMANIUM ALLOYS MADE FROM PROCESS A METAL 0713667—— te 68 , Similar data en the structure of binary titeniumnickel alloya, vontairang up te 10 per cent nicked, are Listed in Teble 17 and Figure 20+ Figures 21 to 2h, inclusive, show typical structures ebsorved dn these alleys. : e fe indicated by Figure 20, nickel mariedly Linite the alphe field and lowers the beta solvus ne, at 1)50°F,, the limit of the alpha-~phaso field is less then 1,75 per cent nickel and, as indicated in the diagram, provetly Less than 1,0 per cent nickel, As 4Llustrated in Pigure 24, 2 nickel-rich phase ({) appears at 7.5 por cent nickel when quenched fron 1,$0°F., but 4s absont, Pigure 23, fn the specimen quonched fran 15S0°F. Fron the availabié date, the eutoo told composition is placed betwoon 6 end 7 per cent nickel in Figure 20, As Indicated previousty, the data do not justify further Anvesti~ gation of binary titsniun-germanium or titaniumnickel alloys. Deta for binary cLioys of titanium with silver, beryLitum, niv— contum, colunbivn, and tantelum are listed in Tebles 18 and 19. ‘Titanium-Silver ALloys Jn the Summary Report, Part IIT, alloys containing 1 and 2 per cent silver were considered. The range of silver content was subsequently Ancreased to 2.5, 3.5, and 5, per cent, rH e BATTELLE WEMORIAL INBTITUTE. opty ,“961 OBed “TTT qes = axodon Aameamg voxy wey ¥yOT ae roRDY YOTATEADTY SOVBOTDUT A a b whed whe d abtd ahtd aed aed = ah +d 6570 620 WO HTT BA O“OT mata ¢ dooowked wed shed wed wed wed = = - - TH O"OT LECH a 4 ¢ é downed hed ded = = = = Se Trem t a d ‘¢ 4 d geo deo gem > 5 ~ 5 + ors Fen > St $y d é d dea gen d+> g+p = - = = WSE sre ‘ sB- ST 09-07 0S ~ 0 oF = oF a é 4 gd ofeo geo deo deo = = = = WSR greAK > OF oF = 09 ¢ g d gee d+2 geo dev deo - - - - TH SL'T LICRK 08 - 0% OS = 0S OE ~ OL \ ‘ *HoOSLT “A OCLT “OSST “L009T *L0SST “0671 “do05L- "84H 7 “eoe7T St 1 a Popueyur *oy : PeGweXL poRvosL poysoss poyver, poqvesy pay2ox, ‘polly a ao, goog yao geen! ymeg! eon deen” porter potter ee a) —_ yon sy 30H BY ugVE TWIN V SsudoE - GAEVOLONT STENLVETOTL LY ‘ SAOTIY THOINDWEIL NNT RI INEST SUSY “LT TTEVE Ab gira eae~10- | O ALPHA PHASE {ALPHA + BETA t pW BETA | | BL BETA +GAMMA\NICKEL- RICH | i | PHASE) : j t i 1759] o_2 2_e——-8 a b i > | : 1700 ee . Lg! ' § : * . 5 16 22s —s 7 ote = 5 / a3 BP Pf 2 i = L | { 1600 tae 2 . o i e i i Ee E & \ 15 | a+6 Bry | 14501 0 10 20 30 40 50 60 70 80 9.0 100110 120 NICKEL, PER CENT ? FIGURE 20. TENTATIVE DIAGRAM SHOWING TRANSFORM- ° ATION RANGE OF TITANIUM-O TO 10 PER 4 CENT NICKEL ALLOYS MADE FROM PROCESS A METAL. oa as rey 9 4 : i ome - 0-13668Figure 21. Heat THiS, 3.5% Mi, Figure 23. Heat “H2tl, 7.9% Mi, - Guenched frem 1600°F. in the beta Quencked fron 1550°F. in the beta field, acicular alpha (transformed field. The nickel-rich phase, show beta) is chow. in Figure 2h, is absent when the epectmen is quenched frem 1550°F, Figure 22, Heat "H2lS, 3.58 Figure 2s Gusnohied fram 1550°F, in the alpha + beta field, Islands ef alphs (ight) 2ppetr dn ex coleuir pha (transformed bata) netrix, Heat “HLL, 7.53 My Suenched fron Lu50°F."in the bata + gemma field. Zhe Light-colored con stituont is the nick-l-rich phase in bets aatrixy Typiosi strastures observed dr binary titintumnickcl slloys 21do" from Process = satel,. > {HNL 29, Euin-reedr 480 A0TH0 DATA OH BISA ALIENS CP ¥ {Ttusny Yi stare, seecx, SOHC, LINDE, FURS PHRPIAED PCE PROCES 4 MEAL hw 2 oe ay si ae i ans us She wie 3M she As v8 as Se 6 x te out >t ae Ms ane 4 son = od DAs Sas ahs 6 we ove Ke wae oAe 3s in ‘TABLE 18, PROPERTIES. CP RIMARE ALLOYS OF TITANTOM WITH SILVER, BERYLLiuw, ZINCONTDM, COMMA, CF SMNTALEM PREPARED! PROM PROORSS A. METAL. 4 -4 eee SRaSE 94,700 Footnotes on following pase.oe SMR MRE Footnotes for Table 184 (1) as hot relied at 150°, (2) Hoterclied sect aged 4 hours at 750°F, in air and air cooled. (3) average of two longitudinal Uegauge specinens, 3 inches long by 04375 inch vide with a 0.250-inchawide reduced section. (4) lovkg. toad, Hardness at the center of the cross section of the sheet 90° to the surface and te the rolling direction, aaa ok MEI Sint es (5) Yinimun bend radius without cracking on a single Longitudinal ‘specimen 3 inches long by 0,5 inch wide. Tested with surface skin presenty * Gone ductilitys ae Very Little auctility, } 2 : ; Ae ALAM ONO¢ SS TENE SM a Pm Footnotes for Table 19: e) wd ) (6) (a) @) @ Qo) ‘Weis. load. Hardness t the center of the cross section of ‘the sheet 90° to the surface and to the rolling direction. Minicun pend radius without creclsing on @ single longitudinal specimen 3 inches long by 0,5 inch wide. Tested with the surface skin present, as hot rolled at 1Ls0%F, Hoterolled sheet aged l hours at 750°F. in air and air cooled, Heated 1/2 hour in air at U4$0°F, and quenched in cold water. Heated 1/2 hour in air at 15S0"P, and quenched in cold water. Heated 1/2 pour in cir at 1600°F, and quenched in cold water. Heated 1/2 hour in air at 1$50"F, and quenched in cold water, Hosted 1/2 hour in air at 1700°F. and quenched in cold water. Heated 1/2 howr in air at 1750°F, end quenched in cold vater,ae ravens a ee ~The : Uechanical Properties. The mechanical properties of the three titaniumsilver alloys, mentioned previously, in both the as-hot-rolled condition and after aging the aschot-roLled temper far hours at 75°F, aro) Listed in Table 28 Figure 25 illustrates grsphically the effect of silver on the tensile properties snd hardness of the aschot~roiled temper, As shown by the data in Teble 15, titaniumativer alloys in the ac-hot-rolled condition do not respond to an aging treatment of i, hours st 750°F. From the prezont data, and the results previously Lsted in tae summary report, it is comiuded that silver, in amouuts uo to 5 per cent, is 4 relatively ineffective alloying addition te titanium Structure and Transformation Renge, The structures obscryed in jitaniumsilver alloys quenched fron texperaturas of 150, 1550, 1600, 1650, 1700, and 1750°F. sre listed in Table 20, The phase relations are shown graphically in Fiure 26. In this figure, the data previously Listed in the sumary report fcr a2leys containing 0.87 ané 2.12 per eent silver are included, It is evident that silver retses the bota and lovers the alpha selvus lines. ztment. The Vickers baranesses and bond characteristics eat of the 2.5, 365, and 5.0 per eent silver alloys, after quenching from Yenperatures of 1150, 1580, 1400, 1650, 1700, and 1750°F,, are Listed 4n Vable 19, At the higher quenching temperatures, slight increases in nard— ness rere obtainud, but there is litte evidence to indicate that titantum silver alleys respoad to solution heat treatment, Aging the asenet~rolied adloye for li hours at 750°F. did not increase the hardness. BATTELLE MEMORIAL INSTITUTE2 —+ ! ® i 2 | : 8 coo page fo . 1o0 }—+ - 2 | & } 2 Zo + > t | Id 4d AS-HOT-ROLLED TEMPER | @ NOMINAL SILVER CONTENT © ACTUAL SILVER CONTENT 1D AVERAGE PROPERTIES UNALLOYED_| t TITANIUM | jot i g 40o[>-——4 [4 E. a | 8a 120}—+ - 4 t—t a t T t ct wee | \ : a8 G : # 1 i 7 1 ! * | pT bo 2a z ox ; ! i ¢ bz I a i i Be gh ~ 0 19 20 30 40 50 E SILVER, PER CENT - FIGURE 25 EFFECT OF SILVER ON THE PROPERTIES OF AS-HOT-RCLLED PROCESS A-TITANIUM SHEET 0-13669"16 aed ‘Try ase ~ socio Axmamg woay uaTe WIG « 4 a g+p dev grep oo > 2 vos - ~ By ots © 9se1 09 ~ oF DY = 09 : 4 d g+> geo geno . . - ee av gE seHN OL- 0 OY= 09 $= 6 a doo de> geo geo ov 2 » - = = = Bye ¥seHH 07-09 0f = O4 of - 06 god g+ > geo geo geo . - p00 Soro zor AY aT AYO" «960N $ 56-5 06-OT cz-08 $= 56 d a g dro . 2 - 2 eto Seo" €o"0 BY La‘o BVO*T #v60K or - 6 8 4 do og+y den > - B otto 92070 0"0 pefotpoun «Lon st-s2 $= 96 ’ ROSIE NHOQUT "HOG “LOOP “HOSEL *UOSYE “asOSle Soma Y “HOR Ko pepuegur “OH ! Pojves, peives; peiuoss pajvedl peqeenl peiwed; pay Eee a1 goon quot gent geon” yw awa portey petty ————— sae RSIS — SoH ev 30H 8y eee wove IVIG1 V SSHO0WL ~ GLLVOLONT STUER LY SSOVIV TMATISHAINVELL TNWNIG A SIMST SECA ‘Ox STEVE e bil 3h, Sama 8g -—O}-—.0- — TEMPERATURE, °F. Shee i -— a |.O ALPHA PHASE | TB ALPHA + BETA | BETA PHASE __ 1 tod bolo 4 | i | Gu |. 0 20 30 40 50 SILVER,PER CENT FIGURE 26. TENTATIVE DIAGRAM SHOWING TRANS- ' ! y args § FORMATION RANGE OF TITANIUM-OTO 5 PER CENT SILVER ALLOYS MADE FROM PROCESS A METAL 0-13670ne fon eS See, ‘taniumeryllium Alloys: Previously, in the sunnary report, titaniun-beryllium alloys con— taining 1.0 and 2.0 per cent added beryllium wore considered. At 2.0 per cont borylliun, a beryllimn-rich phase was noted in specimens quenched from ‘temperatures ranging from 1,50 te 1750°F, Alloys with beryllium additions of O41, 0.15, 0425, 0.5, and 1.0 per cent were Erepared, Wechanical Properties, he tensile properties, hardness, and bend characteristics of the berylliun alloys, in both the as-hot-relled condition and after aging the alloys in the as-hot-rolled temper for l hours at T50°F,, are Listed in Table 16. Figure 27 graphically i1lustrates the effect of beryllium on the tensile properties and hardness of as-hot-rolled titanium shect. In tiis figure, the data previously Listed 4n the summary roport have been included, Perylliun produces no marked increase in the strength or hardness, but progressively decreases the ductility. As will be noted Srom the data in Table 18, the titaniun-boryliur alloys in the as hot-rolled tenper did not respond to an aging treatment of hours at 750°F, Structure and Traneformation Range. Specinens of the titantun veryLliun alloys quonched from temperatures ranging fran 1U50 to 1750°F. were exanined microscopically, Beryllium appeared to Limit the alpha-phase Field and raise the beta solvus Linc, but the limit of solubility of the berylliumrich phase could net be established +ith ay dorree of accuracy. Further study of these alleys will be required before a tentative phase @iagrar can be constructed.pore somes nme. elon rene et na a NR ES, ‘ -19- 2 8 uo 2 6 ca a = 2 © w x 8 i - > oO _! + i \ [-—— AS-HOT-ROLLED TEMPER @ NOMINAL BERYLLIUM [—-— CONTENT | OG AVERAGE PROPERTIES OF ' “FT UNALLOYED TITANIUM = e 1 ° T F Be | | | Ee coo r Bo i { a us e a g Fa é 38 ee g- Zz a o 2 QO 02 04 O08 10 2.0 BERYLUIUM, PER CENT FIGURE 27. EFFECT OF BERYLLIUM ON THE PROPERTIES OF AS-HOT-ROLLED PROCESS A TITANIUM SHEET. 0-13671ain TR Be Heat Treatment. The Tic! -g hardness values and bend character- ishies of the titaniun-berylLiun atioys when quenched fron tenperatures of USO, 1850, 1600, 1650, 1799, and 1750°F. are Listed in Table 19. Ab the e higher quenching temperatures, some increase in hardness was obtained, but thero is ne evidence that these alleys respond appreciably to heat trest= ment, Ae shown by the data in Tables 16 and 19, these titaniun-berylliue alloys in the es-hot-rolled temper de not age bardens ‘Titaniumzircontun Alloys Additions of 140, 2.5, 3655 540, and 10,0 per cent zixconiun wore ade to Process A titanium. These alloys are considered in the following sections Mechanical Properties, The tensile strength, clongation, ye raeion hardness, and bend characteristics of the titeniun-zirconita alloys in both the as-hoterolied condition and aftar aging the alloys in the as-hot-rolled tomper for hours at 750°F. are Listed ix Table 18, Figure 28 graphically illustrates, fer the as-hot-rolied condition, the effect of sdrconiun on ' ‘the tensile strength, elongation, and hardness. Zirconium raises the tensile strength and hardness with relatively Little drop in elongation. “ith 10 per cont zireoniun added, the tensile strength inorrasea about ‘ 37,000 Deeds, sith 6.0 per cont drop in elongation, As compared to chromium, manganese, molybdenum, ani sozs other elenents, sirconiun te : a relatively ineffective alloying aaastion, nese, DATTELLE MEMORIAL INSTITUTEem ete mes OF 5 RON NIRA ro T T : | \ 400 to 2 fd a tod 2 300/— “jot i a £ 200¢ @ fo 4 8} 100)—-——— p= — boop * y Y * s PP = 0 AS-HOT-ROLLED TEMPER —t | @ NOMINAL ZIRCONIUM CONTENT! | © AVERAGE PROPERTIES UNALLOYED 7 fo . | TITANIUM i a py Pir i L | : fori Lf z | poi ' 2 ® 140 joo . 2. i pot 25 Ce | ! be 120 - ; + w | 38 100 3 2 : a f b » f 88 2 e 32 i Bz ? i ge £ 0 10 20 30 40 50 60 70 60 90 100 i ZIRCONIUM, PER CENT 3 FIGURE 28. EFFECT OF ZIRCONIUM ON THE PROPERTIES OF AS-HOT-ROLLED PROCESS & TITANIUM, SHEET o-13e72PRR mtu me -————_— 825 ' As shown by the data in Table 18, the titaniis-sirconium alloys are not appreciably bemefited by aging the alloys in the as-hot~rolled ‘tamper for l hours at 7507 e Structure and Tranefernetion Ranges ‘The phasss present in the titaniun-nirconiun alleys when quenched fron temperatures of 1450 to 1750°F. are Listed in Tate 21, and are shown graphically in Figure 29. Zirconium Limits the slpha-phase ficld and lovers the beta solvus Line, No zirconiur ich phase was cbserved at concentrations up te 1 per cent zirconiun, Hest Treatment. The Vickers hardnese values and minimum bend radii of these titaniumzirconiun loys when quenched from temperatures: of 150, 1830, 1600, 1650, 1700, and 1750*F, are Listed in Table 19. Some Anerease in hardness will be netad after quenching the alloys from the ceed higher temperstures. Horever, the change in hardness is not comparable to ‘that observed in sone of the other binary systens. Aging the as-hot-rolled titaniun-sirconiwa alleys for ii hours at 750°F. did not produce any increase to hardness, It is, therefore, concluded that titaniva-zirconiun alloys in the range of conposition investigated do not show any significant, eee tere response to heat treatnent or aging. EATEN TI PN BATTELLE MEMORIAL, INSTITUTE coe See 2 Nm a AEE4 4 d é de> gee dre tee 3 vot ores Of - 04 OF - 04 boo | d dep! g4+0 geo deo dee 4z0rs * Oseun 05 - 0S . 4 d de> deo yao gemen 2 > a ste sen ‘ OL = 08 OS ~ 0S Ot ~ oO d q der d+ > geen 2 » > az st 2S2HN 4 Pr a d dee deo 2 2 > . 32 O°T een oe oz “oe ‘ d de> deo geo gryen! 2 2 peforroun grein | of-0L of-~08 OT= 06 } “Se OSLT do 00LT do OS9T “do 009T "i OSST. OST "do 0SL=*84 OST f ‘uoTyFEoduog “OH 98eH : Pequot, paqwosy pequary ‘poqwery, ‘poqwory, ‘pozery, ‘poy J ‘pepusquy Ea a verte 1 90H By 7011 BY i SS Sve TYLO ¥ SSHOM - CAIYOTUNT sMMINEOME Lv SAOTIY MATNOOUTZ-HATNVITE AMWNTO NI INRSMLE SESVHI ‘Te IOV Deiat uti toinesinin ai tester in abdabliiddnieciaestdass deesy1 ate REE NEP oye ROE ETE NETE IE. en er =the Tt | | © ALPHA PHASE | . | ALPHA + BETA © i @ BETA PHASE | | | | 1 ' 1750, +— : . al ° | 1700) A= fe Bf oP * 8 Up 1650} 28 wy —? @ 2 | ™ 3 | PSN Q | | £ too a SH - i Pop NY Bos a | | ! 4 H | hot | 1380, Soo ' : it No Poi 4 pybopod on H (500-4 rT \— 7 ft 4 ot : | || ' yl i ; 4 1450L__9—__Lo. Ay Lot e 0 10 20 30 40 50 60 70 80 90 100 ZIRCONIUM , PER CENT FIGURE 29. TENTATIVE DIAGRAM SHOWING TRANS- FORMATION OF TITANIUM-O TO 10 PER CENT ZIRCONIUM ALLOYS MADE FROM PROCESS A METAL 0-13673be 1 8 me ORE A pmo Soe at Sein AEE SERN IRE B 8 ‘TteniunColumbium Alloys Additions of 1,0 and 2,0 per cent columblum ware made to Process A titanium. The properties of these alloys are considered in the following section, Jigchanical Properties, The tensile properties, hardnesses, and minima bend redii of the two titenium-cclunbium alloys, in both the a hot-rolied comlition end efter aging the alleys in the as-hoterolled tesper for h hows at 750° are Listed in Table 13, Figure 30 graphically illustrates the effect of colunbiun on the as-hoterelled properties, The tensile strength and hardness Snerease with increasing colunbium content, hile the slengation decreases. These two colunbiun-containing alloys id not respond when the as-hoterolled sheet was aged 4 hours at 750°. Considering the above properties, the range of eolunbiun content wiTl be ertended to 10 per cont. ‘TitaniunTantalun Alloys Alloys conteining 1-0 and 2.0 per cent tantalum vere investi- gated, The propertias of these alloys are considered in the following seetions Mechanical Properties. The tonsils properties, hardnessos, and ‘ininun bond radii of the tvo titantun-tantalum alleys are ilsted in Table 1B, These date are for the alloys in the as-hot-rolled condition and after aging thr alloys in the as-hoterolled tenper for h hours at 150°F. Figure 32] BATTELLE MEMORIAL INSTITUTEJP z & 4 L040 EIRENE NP SHE PETAI a PET TERLT SP Rn 100] : = VICKERS HARDNESS AS-HOT-ROLLED TEMPER A @ NOMINAL COLUMBIUM CONTENT |_ ( AVERAGE FROPERTIES | UNALLOYED TITANIUM | i | 8 TENSILE STRENGTH, (000 PS. 3 rs RT ‘et. ‘e-- % IN 1 1N INCH 20! od ELONGATION 0 16 20 30 40 50 COLUMBIUM, PER CENT FIGURE 30. EFFECT OF COLUMBIUM ON THE PROPER- TIES OF AS-HOT-ROLLE'D PROCESS A TITANIUM SHEET 0. 13674Ds VICKERS HARDNESS ° EW aa PO TTR {000 PS. |. TENSILE STRENGTH, ELONGATION, % IN} INCH fof. : AS-HOT-| ROLLED TENBER @ NOMINAL TANTALUM CONTENT. FG AVERAGE. PROPERTIES NAL LOVE} | TITANIUM i po 4 : t ; 20 tg ++ po 4 10-20 30 40 50 TANTALUM, PER CENT FIGURE 31. EFFECT OF TANTALUM ON THE PROP- ERTIES OF AS-HOT-ROLLED PROCESS A TITANIUM SHEET O-13675re ER I cen pays oe hehe FST dd AOR ENE 88 graphically iMuetrates he effect af 1,0 and 2,0 per cent tantalum un the tensile properties and nandness of Process 4 titanium tn the as-hot-rolled condition, The addition of 240 per cent tontalum increased tho tensile ctrength of Process A ti- taniun shoct about 20,000 pe set. with a reduction in clongetion of about 3.0 per cents additional data on binety titaniun—columbim and titentuc-tentalun alloys, when the range of Rle ‘#OOTSTRT Tety *O°T ‘#00T'2TZ «= OTs aw ” . ote ‘ol fogt TH OT ook titz apes tery got 008*L0z, $2 sda um eysag —goquep Sot oogiet = st xo «wea ou x008'S6T SEO F20Z apts tauoa yeh mee 009 HET TEKS. 6a OT oe zz~ — PPTs "guead a30°z*OSZ"0" 100"S T-¥ apy ‘aeey yoy uO? ose yy TE seed eR usp 4 EK ‘Spys uo oy a wax & apts ‘quotg ogg*2‘OSz"0'A05"C TX gut ree ooz's2 “Bay Zt orzz 00 oye ‘sao » zs « LT 0°88 00‘ S) OpTs “resy a T a ge Ortz 0005 dequag uw ok ” T or€2 —ongfS ——_gaquag * TE * Blt 0f8e 002. 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B09 06ST eps ‘azo, ™ 09 oogtgdt enue 2 O'S os tgLt —aeaueD ” on cog tat apts suas on ox » O°] OOK FALT apts“ quosg S62*0°URS THK ON our (z)*pterd — wowyoody z soy “OH tire “fighens 30 ‘aoyyysoduoy —roedg HoH “Burr — styoumy —worveoo1§=——pabuegutyope StS OOttelt “Baw Toi Ors opefogt pts ey ele OS cog fogtT = epTe*ey TE GE oF ok ght xagteg he ee 6s 09 contLit soy. wow ow OE = ~ Sn - - = eppeyuoss — warofnO*TSA00°S THK sue are 009‘ Tst “Bay « ey oot ooni9st opr ieoy « ae * ole On oopsst apTeSreey tt HE OTE oot soquan ® wk “ 3 ale ont oostzét angen * ta “ e wt OT oog‘TeT sprs‘quoay on a Xk 0 ee ont oop'set SPIE GuOTE OSerotROre“HO0"S TX wn guest oostret ‘Saw SUE wOrSwOORFELT opr arer nw ee gle 40'S = Q0OCSLT pre ‘rey be om Ons O0g‘LLT = tou. » aK ot Tee ont 0094ZeT oyu a eK “ oe Oth OOStLgT RFS tquom; aK . ze ot Ong LET SpTB‘QuOTy — 0 L“UNO"S TK ost. (6) your (gytyrerd sey (€) u(y tfretd = uourpoods: £ som sen A cur g “fvmens yeeH meh LUE ¢ HegSuezas Jo fuotyzboduog —0edg a Sue ‘eswTT —STFSUOR—uoyauooy | PapusquT, (Heuer FOTN Buysn pesedear SxOTT (UATE) "ye BEVa ene SS aps “00H a opr Seay Ta Tae ca. 53129 Tx ‘epTs “uOKy ax i opts ‘quot Tx 1 for otk oop fast “Bay ! Ege one 008591, opis ‘rey ee » | eof 0D. MOOT’ AT ‘pts ‘ze0y te o gst 0rLcagtdSt © segu0g wa . an otk cotgt_aequeg Tk * 1 Lu oF OOS*EST © spre‘ quoad aK a 24 TEL Og COSFEST epEe quae TK eh H ozs ‘srey ae : apts ‘270u re sous an 4 oye9 TH & aprerquoxg zx - apse Quod Te Tee St DOL fogT “BAY Len on ood “HgT opts ‘away 22 a Tey Oo ggT PFS “ava 1 “ WE om / 00g seque a ™ mE 0"9 OL‘ELT — seaua9 Th “ LIE 0S Om tzgT opta‘quos zx . 6 so] MOOTSGIT OPT Rua TX Tha (e) uur (gyeretd son (ED goer (gy*revd —uewtsedg ‘ voy 8 wth try “Mpduog eer mia TTS Rauaayg Jo fuorstoadiog —*o0dg 80H ‘emota — eTeuay —wortesoy © popuoquyve PEROG A SOR Ym connate 4 ay ri * * ssduyprer G 4eeeT qu Jo aBeTOAY “BUTTTOI Jo woTIOATAD avy OF PAE soLyaNE 243 04 06 wPEPImdS sTTSUOy gooye aia Jo UOTIOeS aeoda o4y Jo FoquIOD ayy ge EHOUPIUH “Peo "SHOT 3 pe OL COST — apts ‘reay so TE ‘ ; 69° ond OTST = xequag, ow ak iy ee OL cog*ygt se qusp 4 1 ' dc 09 costsit epra‘woas ie 2X “ | ole org COTGT spre‘ guozT OZ HSE TX Lat : (2) aur pystd toy (€) su sped uourosdg 3 son “on BA vrs FRas wy Gk tay Rektome “Se? tuopeyfotneg sds en t “ 25 aA 4 é uoyarooT = Pa uEAUT ant (pssuepren Aor y Buysq poredaag Shorty oa (canNtiwoo) “2 Etave96- “ IVESTIOATION OF REFRADTORTES FOR MELTING TITANIUM (Fs D. Maddox and L, % Bastawod) ‘The investigation of refractories for nelting titanium was cou e tinued. Folleving the previously established practice, 10- to 15-gram nalts were made under an argon atmosphere, After cooling, the melts and crucibles were sovtioned and exanined. During the pericd covered by this report, the evaluation of the noite nede in the tantalua carbide- and tungsten berideLined oarbon cru- cibles vas completed, Additional waits were nade in hot-pressed titanium carbide, hot-preesed uiroordum oxide (stabilized with 020}, caletwn oxide, calcium oxide (f'luxed with 0p}, ant aluminum oxide crucibles. The last : 3 crucibles, made by compressing and sintering, had porosities af 146, 08, and 1.6 per cent, respectively, The hot-pressed sirconiua exide crucible was wet by the titantum in only one place, However, the Vickers hardness inerensod fren 160 for the melting steck to U0 for the melt, & survey of the melt showed that the netal near the point of wetting was LO to 60 Vickers mmbers harder than ‘the rest of the molt, Wo hardness values below hOO were found. Tt iy therefore, ronotely possible that the hardiness increase may have resulted from contaminetion introduced at the point where the titaniun wet the e erucities ‘This sireoniun oxide crucible will be examined to show variations . . in composition or structure if any oan be detected, Since this is the first rafractory matarial which had areas not ret by the titantur, further ex~ perimental vork <1] be carried oat to oxplere the refractory fully, BATTELLE MEMORIAL INSTITUTE,oa Examination of the melts made in caleium, oxide, otledun oxide fumed swith 2 per sent Md, and alusinun oxide crucibles shows thet the Mguid titentun reacte with these crucible materieis, lardness measure onts vill be mado and they should Sndinste the extent of the reactions ‘The results of tho prosent experimental vork are summarized in Table 254 © Ba Rack ie le ANALYTICAL METHODS FOR TTWNIWueBASE ALLOYS Studies on the Chemical analysis of Oxygen in Titantun = ecarbon Tetrac el (E. J. Center and a, 6, Bokert) Jn the previous bincnthly report, there vas a trie! discussion of the chlerine-carben tetrachloride method for determining oxygen. It was indicated that a detailed description of the apparatus and techniques used dn the investigation of this proposed analyticel method would be inoluded 4n this report, The follaving section coutains these data, Tt was suggested that. the decmposition of titantun ty a mixture of carbon tetrachloride and cticrine might sarve as the basis for a deter= : ination of smal quantities of caygen in the metal, Treatoet sith this gaseous mixture should distill the titanium as titenium tetrachloride, release any free oxygen present, and convort any combined oxygen to carbon monoxide or carbon dicxide, Passage of the products of this reaction over hot carben should convert all oxygen to caxbon enoxide, hich could then be eellected and analyzed by conventional methods. This proposal. was based on repertad nettiogs for the determination of oxygen in argante coapomnte(?) ‘together with the suggestion thet the carben tetrachLoride-chlorine mixture should readily decompose titanium wotal and titanium oxides st moderately BATTELLE MEMORIAL INSTITUTE,cuoyyoe Supuyyeeuyesd » am 04 sxvedde pue seTTEUE YOR ef quemaTAEUOD OW ‘aasanoy Squosont sya ‘soTaTonio opyqiwo Uy ape ep Teu 07 solwsuedde UT uMTTES fxn ‘oeeyd puOsES ¥ (S) seydues yy gnoydnoma peynaTeTp ATuTOspUN useyed OTVTAplep E UT SxEedde osuyd aprgara oul i SORT, Sem epeu sea oO4e ZuTaTSM pospoAIOS ayy YoRY Woy AORUT unUEYTT a¥y Jo sooIpTEY suNOTA CC} wg. AUMBTTS ssouneEY ayy 200T PTHOM Feq PEBIOS oly RuyaTos “Posmnaeo WopyeUTBEAWOD OM IT Tepe | ‘adda sgo8uT 4804 ayy GOYA UOTZEUTWEZUOD Aq PATILO OLE STN4 Uey2 acqwad genyea ssoupsey ‘kT quanboslon “OUe 4ek opew sea seens MUTOH pos-petsey ees wopNR MOAT aH MRIMENT Jo Saevpiry SuNIoTh (2) syouy Jo doy uo cnazquew £q poqzopelT (7! etazonto Jo "1 ~ Aavpo0d see qe awos eqeth0o 4oN, = epye au uo 4%, woBay —fpassnaduos Eoty 59°0 ~ Syz90a0d arqyono fpeasusdwos (Orr, sioRg9U owog enetdaoo yon = Jo ceyoueyp 2/7 98. WORAY —#z UNA PoxMTE) OLD 1 prt — Ayywosd Qo yeeyte aug ‘eyetdwo 30N — Suyyzee oras TT Auea — woB ay ‘fpesseatiwos~o¥) . (080 WATE pemeran outa ‘eyetdwos yon «eon ~ gods ou uy Sup woRay “” Zp7 papsesth4o} eragone oy ovta & eyouqcos meg (2906 - sex woSay -ydea? wo SuTUsT es : sTaqroRe egzydesd uo ont onan (ise - or uoSsy — Suyury Aavey ged ! oem ia awserae xoenae ox opstlte eraempsu —(4y692 2 ano 9K wo8.y ‘OEE pesseatyoH eoegroqur wovaeururm — (peoTBu-o1) ‘STeATENY —(q) TL dq etoudsony Teraeqe Lxoqowsjou-r ye opydusBoT TEN —’ssoupreN—TeaTUAYD ‘atarazg BUTTON erasonag ‘orqay eTazonIg 820H0TK p SuT199,, CENTYZAO SUINSHE GRY GULL SUTMOLOVUIH RO VEE “$2 THEE= high temperatures, : ‘This investigation shows that such 2 method involves certain Siffloulties which wake it Ampractical, a variation of the stethod based on Aistiliation of the titanium (as the tetractiloride) by treatment ith chlorine followed by chonical anslysis of the residue 2190 appears to be Ampeactioal ‘ThSs investigation consisted in first finding satisfactory materials for construction of the necessary apparatus and then finding @ set of conditions undor which decotpositien of the sample weuld ran to & sulficlent deyres of completion. Figures 32 and 33 show a schematic drawing and a photograph of the apparatus, Tho purifying train vas constructed of Pyrex glass and Tygen ‘tubing ani the coninstion tubs was nade of fused silica. Fusod cilice ant ceramic Leco-Type HPO bests wore used to contain the sarple. The various samples used included both Burean of fines titaniua ponder and Du Pont ‘sponge titanium, Table 26 gives the typical analysis uf the Burea of Wines ponder, fable 27 sumarizes pertinent information concerning the runs ade, % In otéer to chook the general operation of the train and furnace, a nunber of qu@litetive runs were made. These runs are not included in fable 276 BATTELLE WEMORUAL INSTITUTEi Picdeainianiieinics aie lieti ed La SBP Si : sro NIVEL NOLIVNINOTHO ONIMOHS ONAVHS SLWWZHOS Ze SuNos 2H BED) », i voIs ‘TOTIV9ONAd 199 Ve Posty : if. 4 * ~ ~0s?H I [ Jvoe aTawys : } ’ Ic a . Py PFE SS} ~ ' via 49 3 tanooonwaH f auiwaiya 7199 109 Posty *19090 . BovNUNS os (I li “T13M 31dNOSOWH3HL- , 4 } | 4 SY. al Elna atta cine cease=e TABLE 26. TOPICAL AMWLYBIS OF BUREAU OF MIMES TUTANIUM PODER Blement, In Table 27, 4t 4s evident that the decasposition of the sample yas never better than 99.7 por cent, except when temperatures above B00°C. Were used. Although the residuos of these Migh-tecporature trestacnts are spproxinately 3 por eent of tho sample treated, they ropresent Less then ‘vo hurtiredths per cent of the original savple, since they are residues fron ‘titeniun metal decompositions whist took place st lover tenperatures, This tmo-step prosodurc “26 used because it vas found that the heet ef reaction of the Dulk sample wos so greet that it was GLffictlt to avoid cracking the boats. in order to have © weighatle quantity of mterial after the high-temperature troatmont, it vas necossary to start vith a Large quantaty of original sample, Because of physical Linttations, it nos generally more Convenient to perform the lover tenperature decompesition of this large quantity in several swaller betchens : ‘The results recorded in Table 27 shox that, although the de couposition of the sexble wes sufficient at the higher temerstures, = ‘Significant anount of attack took place on both Kinds of teats divastigeted, BATTELLE MEMORIAL INSTITUTE ae103+ TABLE 27. SIMMIARY OF RUNS Boat Con . on sumption, . Now ug 1 5 2 450 2 Tate 8 3 450 4 " 7 8 (2) 4 525 5 . 2) . 5 55 eae " 373 # (2) € 525 bafe " 0.9 Q) GQ) z 350 1/2 . 0.8 o 8 550 a-1/e . 2) 9 550 pie Du Pont sponge 0032 10 575 1 Bureau of Hines pomder (2) cre 6 7 Ditte 65k, Bb 2» So 5 . ae 3 @) 13 oS a " one co) uy 6 bafe 05, 126.3 Td a0 3-2/2 Residue Run Nos 6 27 26.2 (3) 2 So a Residue Runs Nos, 9, 343 26.4 (3) 9 23 u on 6 Residue fun Noo 12 hh 2h Q) 0 cy, sed, (2) Boat cracked’ during run (3) Lece HF-C beat used.sil 101- ssmiededdy aun so qe~1ole Since the attack on a eflien boat prebably involves 2 reaction in which oxygen is relaased, as carden monoxide, At is likely that the quanti ay exelved from the wells of the ica corbustion tubs woutd cause an ox~ cossively Ligh oxygen blank in an sotusl detersination, | Corre thon of results from spoctrographic and X-ray diffrsction anslyses of residues fron the lover temperature reactions indicates thst the: nixteniale consiet essentially cf spinels. Gniy 5 trace of quarts As prosent. Magnesium 4s presint, principally ag magnesion oxide, although At Ls possible that som of it is ac tituent of ene of the spincls. No oxide of titsniue is found, although sons of ths spinvls possibly present cortsin titanium togvther sith oxygen in the ratie of 1 or 2 oxygen ators per titeniun stem, Bocwis. of their clos sintlarity in structural arrang: niont uid lavtics constant, individual spinels evsrot |. distinmishou or gy ovidines.” The oxietine the spins is pretaey, widrlring Pieter in micine dovlopnert of tm omilytied rethed dittieult, sie tg ore extrem: and einer?) aMrficalt to capos « lichurcer fousd that dr. street of ehlerave wt 10.080, fer 39 Hours = sirdiw srdnel Lost only 5 por cont of tte -naghte On the reidu. fron resetbons wath hlerine “ere y eho uek recount for 3 Large peresntage af the 6% wansted teh toana Boowiry mectainty wets os te : nk tis cubdation ot soekate: raait ingore PATTELLE MEMONIAL INSTITUTE,1G On the basis of results discussed above, It is concluded that the carbon tetrechloridechlorine method is inpractical for the determination of small amounts of oxygen in titanium metal because a significant amount of the oxygen is conbined in spinels and, thas, conditdons are required for decomposition t cause excessive attack on tho boat and the walls of che sonimsticn tbe, The chlorine-chesicel anelysis method fats brosuse of the uneertainty as to the Ti-0 relationstip 4n the original sarple and in the chlorination residue, The analysis of Titanium for Oxygen ae acmehas ion ESTO In the previous tdmontiy reper’, the te: que used at Retteile and the results chtained in the anslysie of titaniu, for oxygen by the pated fusion method ere descriles, In the shor» venort, it that sanples of jodie titaniun “rit ‘mom amounts of ry yen added as Tig wore belng orapared and sould be te oa lowne, of the Carnegie » for vacsundunier walysic iz tle lal oratory, on deserives (1) the praarstion of the standard samples, (2) the anvarsius and technique used by try verge, ani (2) the results of ansiveis. PATTELLE WEMORIAL INSHTUTE~106- hm onail capsule of iodide titaniun vas prepared by drilling a Fole in the iodide titanimn, adding a weighed amount of dried C.P. Tit in the hole, and plugging the hole with a machined rod of iodide titanium, ‘The prepared stancard was then deuble melted in argch, Before melting, ‘the systen vas evacuated to atout i0 microns three tines, flushing te about (-cn.pressure with ary, pure (99,95) argon between each evacuation. Then, the systen was evacuated to O.1 micren, and l0-on. pressure af argon was tdnitted, The system was evacuated to Oel sicron again and 10cm, pressure of argon was aduitted. The arc was then struc against the copper crucible away fron the charge. Kelting vas complete in 10 to 15 seconts, after cooling, the button as turned over and the nelting procedure as repeated. Ten standard samples of iodide titanium “ith xnom additions of oxygen aded as Ti0p vere presared in this manners after melting, the specimens vere ground and the Vickers hardness detersined on the top and hotter of each specsnen. Table 28 contains the data pertinent te the preparation of the standard samples. Figure 3h shous the relation of the Vickers hardnese ard the calculated oxygen contest. The correlation be teen hardness and oxygen content sho.s renarkatly Little variation, These samples vere assignes rabers, as indicated in Tatle 28, ané sent te Dr, Derge fer analysis. BATTELLE MEMORIAL INSTITUTE RE APRN pelt ATS!