Correlating microstrain and activated slip systems with mechanical properties within rotary swaged WNiCo pseudoalloy

ma e ials A icle Co ela ing Mic os ain and Ac i a ed Slip Sys ems wi h Mechanical P ope ies wi hin Ro a y Swaged WNiCo Pseudoalloy Pa el S unz 1,* , Lenka Kunˇcická2, Pˇ emysl Be an 1,3 , Radim Kocich 2 and Cha les He oches 1 1Nuclea Physics Ins i u e o he CAS, 250 68 ˇ Rež, Czech Republic; [email p o ec ed] (P.B.); [email p o ec ed] (C.H.) 2Facul y o Ma e ials Science and Technology, VŠB-Technical Uni e si y o Os a a, 708 00 Os a a-Po uba, Czech Republic; [email p o ec ed] (L.K.); [email p o ec ed] (R.K.) 3Eu opean Spalla ion Sou ce ERIC, 225 92 Lund, Sweden; [email p o ec ed] *Co espondence: [email p o ec ed]; Tel.: +420-266-173-553 Recei ed: 27 Sep embe 2019; Accep ed: 30 Decembe 2019; Published: 3 Janua y 2020   Abs ac : Due o hei supe b mechanical p ope ies and high speci ic mass, ungs en hea y alloys a e used in demanding applica ions, such as kine ic pene a o s, gy oscope o o s, o adia ion shielding. Howe e , hei s uc u e, consis ing o ha d ungs en pa icles embedded in a so ma ix, makes he de o ma ion p ocessing a challenging ask. This s udy ocused on he cha ac e iza ion o de o ma ion beha io du ing he momechanical p ocessing o a WNiCo ungs en hea y alloy (THA) ia he me hod o o a y swaging a a ious empe a u es. Emphasis is gi en o mic os ain de elopmen and de e mina ion o he ac i a ed slip sys ems and disloca ion densi y ia neu on di ac ion. The analyses showed ha he g ains o he NiCo2W ma ix e ined signi ican ly a e he de o ma ion ea men s. The mic os ain was highe in he cold swaged sample (44.2 × 10 −4 ). Bo h he samples swaged a 20 ◦ C and 900 ◦ C exhibi ed he ac i a ion o edge disloca ions wi h <111>{110} o <110>{111} slip sys ems, and/o sc ew disloca ions wi h <110>slip sys em in he NiCo2W ma ix. Disloca ion densi ies we e de e mined and he esul s we e co ela ed wi h he inal mechanical p ope ies o he swaged ba s. Keywo ds: ungs en; o a y swaging; neu on di ac ion; disloca ions; mic os ain 1. In oduc ion Gi en hei excellen mechanicalandphysicalp ope ies, ungs enhea yalloys(THAs)a epopula o demanding applica ions in he mili a y, adia ion shields, and highly demanding componen s such as ai c a coun e -balances and gy oscope o o s. THAs usually consis o 90–97 w .% o ungs en plus o he elemen s, such as Co, Ni, Fe, and Cu [ 1 ]. THAs a e gene ally wo-phase composi es consis ing o sphe ical ungs en pa icles/agglome a es su ounded by a duc ile ma ix [ 2 ]. Ne e heless, he s uc u e cha ac e is ics consequen ly impac ing he pe o mance o he inal p oduc can non-negligibly be al e ed by e en he sligh es modi ica ions o he p ocessing echnology. By his eason, cha ac e iza ion o he occu ing s uc u al phenomena, such as he possible p esence o adiaba ic shea bands (ASBs), de e mina ion o he p esence o mic os ain and esidual s ess, and cha ac e iza ion o disloca ions and ac i e slip sys ems a e o he u mos impo ance. The i s men ionedphenomenonhasbeenin es iga edqui e ho oughly[ 3 – 5 ], bu de ailed wo kscha ac e izing o he s uc u e phenomena du ing de o ma ion p ocessing o THAs a e sca ce [6,7]. Recen ly, se e al pieces o esea ch ha e shown ha imposing in ensi e shea s ain in o THAs du ing hei p oduc ion enhances hei u ili y p ope ies and ballis ic pe o mance [ 8 , 9 ]. E ec i e Ma e ials 2020,13, 208; doi:10.3390/ma13010208 www.mdpi.com/jou nal/ma e ials Ma e ials 2020,13, 208 2 o 15 s uc u e e inemen can p e e ably be in oduced ia me hods o se e e plas ic de o ma ion (SPD), o example ia he widely esea ched equal channel angula p essing (ECAP) and i s modi ica ions, which ha e been p o en o e ec i ely e ine he g ain size down o se e al hund eds o nanome es o a iousma e ials omaluminium o ungs en [ 10 – 16 ]. Ne e heless, he majo d awbacko p ospec i e indus ial use o SPD me hods is hei limi ed applicabili y o bulk olume samples. Fo example, he mos e ec i e high p essu e o sion (HPT) me hod is only sui able o p ocess coin-like samples [ 17 ]. By hese easons, THAs a e mos ly ab ica ed ia a ious he momechanical ea men s and mo e con en ional echnologies, such as ho ex usion [18,19], cold olling [20], and swaging [21–23]. Ro a y swaging (RS) is an in ensi e plas ic de o ma ion me hod ad an ageously used in he indus y o g adually educe c oss-sec ions and inc ease leng hs o axisymme ic wo kpieces [ 24 , 25 ]. Gi en by i s inc emen al cha ac e and dominan comp essi e s ess s a e, he me hod can a ou ably be used o p ocess sin e ed ma e ials [ 26 ]. The dominan shea s ain mechanism enables elimina ion o esidual po osi y and impa s signi ican s uc u e e inemen . The p ima y aim o he p esen ed s udy was o de e mine mic os ain and cha ac e ize he disloca ions and ac i e slip sys ems in he o iginal sin e ed THA, as well as in he o a y swaged ba s, in o de o cha ac e ize he e ec s o he momechanical ea men on he mic os uc u e and inal mechanical p ope ies. Th oughou he pape , he e m “mic os ain” deno es he oo mean squa e o he a ia ions in he la ice pa ame e s ac oss he indi idual c ys alli es ac oss mic oscopic dis ances ( oo mean squa e s ain, RMSS). In con as , he e m “mac os ain” (no epo ed he e) e e s o he o e all change in he la ice pa ame e caused, o example, by a esidual s ess dis ibu ion ac oss he whole componen . Gene ally, mic os ain can be caused by a dis ibu ion o c ys al de ec s such as acancies, disloca ions, s acking o win aul s. Neu on powde di ac ion me hod was used as he p incipal ool o he cha ac e iza ion o s uc u e and mic os uc u e. The s eng h o neu on di ac ion lies in he possibili y o p o ide in o ma ion om he bulk o he sample, no only om i s nea -su ace egion. This ac is e y impo an , especially o THA, whe e he ma e ial is composed mainly o ungs en which is highly abso bing o he adia ion (X- ay, elec ons). When neu ons a e used, he signal is a e aged o e a la ge olume and he e ec s o local a iabili y, la ge g ain size and possible local a e ac s a e minimized. 2. Ma e ials and Me hods The W-Ni-Co (93-6-1) w .% (80.9-16.4-2.7 a .%) pseudo-alloy was p oduced by powde me allu gy. The pa icle size o ini ial W, Ni and Co powde s was in he ange o 2–4 µ m. The weigh ed mix u e o he powde s was homogeneously mixed and hen sin e ed a 1500 ◦ C unde H 2 p o ec i e a mosphe e, andsubsequen lyquenchedinwa e . Theas-sin e edma e ial,i.e., ba swi happ oxima ely 12 ×18 mm2ellip ical c oss sec ions, is deno ed as W_0 h oughou he ollowing ex . The sin e ed ba s we e u he p ocessed by o a y swaging (RS) in o ci cula swaged ba s wi h a diame e o 10 mm. RS was pe o med in wo di e en ways: a oom empe a u e (sample W_A) and a 900 ◦C (sample W_B). The neu on di ac ion pa e ns o s uc u e and mic os ain de e mina ion we e collec ed a ambien empe a u e on he MEREDIT di ac ome e o CANAM in as uc u e a NPI ˇ Rež nea P ague [ 27 ]. A mosaic Cu monoch oma o ( e lec ion 220) p o ided neu ons wi h a wa eleng h o λ=1.46 Å . A small (0.4%) λ /2 (0.73 Å) con amina ion o he incoming beam was p esen and was aken in o accoun du ing he analysis. The samples we e ixed in he beam using a sample holde enabling a sample o a ion along he e ical axis o a e age he ex u e and la ge-g ain in luence on he di ac ed in ensi ies wi hin he di ac ion plane. A neu on beam size was selec ed o subme ge he sample ully in he beam. The di ac ion pa e ns we e collec ed om 4 o 144 ◦ o 2 θ (whe e θ is he sca e ing angle) wi h a s ep size o 0.08 ◦ using a mul i-de ec o bank (35 3 He poin coun e s wi h co esponding 10’ Solle collima o s). In o de o assess he g ain size, an addi ional neu on di ac ion measu emen was pe o med using he TKSN-400 di ac ome e [ 28 ] equipped wi h a 2D posi ion-sensi i e de ec o . This measu emen was ca ied ou wi h he neu on wa eleng h o λ=1.21 Å. Ma e ials 2020,13, 208 3 o 15 Fu he sample analyses we e pe o med using scanning and ansmission elec on mic oscopy (SEM and TEM) on ion-polished ans e sal samples aken om bo h he swaged pieces and om he o iginal sin e ed ma e ial. SEM-EBSD (elec on backsca e di ac ion) analyses we e pe o med using a TESCAN Ly a 3 de ice equipped wi h No dlysNano EBSD de ec o wi h he scan s ep o 0.1 µ m. The subs uc u es and g ains analyses we e pe o med using ATEX [ 29 ] and Channel 5 so wa e. TEM images we e acqui ed on ion-polished hin oils wi h a JEOL 2100F de ice. The las s ep was cha ac e iza ion o mechanical p ope ies ia ensile es s pe o med o e alua e he mechanical beha io o he sin e ed and swaged ma e ial s a es and o de e mine hei ul ima e ensile s eng h (UTS) and maximum elonga ion. Tensile es ing was pe o med wi h 100 mm long ba s and a s ain a e o 1.3 × 10 −3 s −1 using a Zwick de ice. By he eason ha de e mina ion o elas ic p ope ies on ungs en hea y alloys is complica ed by ensile es s due o possible de lec ions o he s ess-s ain cu es, he elas ic moduli we e addi ionally de e mined ia ul asound measu emen s by an Olympus 38DL Plus de ice which applies he Pulse Echo O e lap (PEO). 3. Resul s 3.1. Phase Iden i ica ion and G ain Size P io o mic os ain de e mina ion, phase iden i ica ion was done using di ac og ams measu ed a neu on di ac ome e MEREDIT [ 27 ] o all he samples. An example o he measu ed and calcula ed neu on di ac ion pa e n o he sample W_B wi h ecognized phases is shown in Figu e 1. The o he wo samples exhibi ed simila phase composi ion and he di ac og ams a e simila , al hough hey di e in de ails due o peak b oadening, as will be discussed la e in he ex . The phase iden i ica ion and analysis in all he samples was pe o med by ull-pa e n e inemen using FullP o so wa e [ 30 ]. Ma e ials 2020, 13, x FOR PEER REVIEW 3 o 15 Fu he sample analyses we e pe o med using scanning and ansmission elec on mic oscopy (SEM and TEM) on ion-polished ans e sal samples aken om bo h he swaged pieces and om he o iginal sin e ed ma e ial. SEM-EBSD (elec on backsca e di ac ion) analyses we e pe o med using a TESCAN Ly a 3 de ice equipped wi h No dlysNano EBSD de ec o wi h he scan s ep o 0.1 µm. The subs uc u es and g ains analyses we e pe o med using ATEX [29] and Channel 5 so wa e. TEM images we e acqui ed on ion-polished hin oils wi h a JEOL 2100F de ice. The las s ep was cha ac e iza ion o mechanical p ope ies ia ensile es s pe o med o e alua e he mechanical beha io o he sin e ed and swaged ma e ial s a es and o de e mine hei ul ima e ensile s eng h (UTS) and maximum elonga ion. Tensile es ing was pe o med wi h 100 mm long ba s and a s ain a e o 1.3 × 10−3 s−1 using a Zwick de ice. By he eason ha de e mina ion o elas ic p ope ies on ungs en hea y alloys is complica ed by ensile es s due o possible de lec ions o he s ess-s ain cu es, he elas ic moduli we e addi ionally de e mined ia ul asound measu emen s by an Olympus 38DL Plus de ice which applies he Pulse Echo O e lap (PEO). 3. Resul s 3.1. Phase Iden i ica ion and G ain Size P io o mic os ain de e mina ion, phase iden i ica ion was done using di ac og ams measu ed a neu on di ac ome e MEREDIT [27] o all he samples. An example o he measu ed and calcula ed neu on di ac ion pa e n o he sample W_B wi h ecognized phases is shown in Figu e 1. The o he wo samples exhibi ed simila phase composi ion and he di ac og ams a e simila , al hough hey di e in de ails due o peak b oadening, as will be discussed la e in he ex . The phase iden i ica ion and analysis in all he samples was pe o med by ull-pa e n e inemen using FullP o so wa e [30]. Figu e 1. Measu ed and calcula ed neu on di ac ion pa e n o W_B sample used o phase de e mina ion as well as o mic os ain cha ac e iza ion. The B agg posi ions o indi idual ecognized phases ( om he op W-B2 and NiCo2W; i should be no ed ha also he peak posi ions o λ/2 con amina ion wa eleng h a e shown) a e below he in ensi y cu e. The di e ence be ween he measu ed and calcula ed in ensi y is shown as well. Two phases we e iden i ied in all samples. The main phase is α-W (B2 s uc u e; wi hin he ex , i is e e ed o as W-B2 phase). The second phase wi h a weigh ac ion o 6%–7% has pu e-Ni-like s uc u e ( cc) wi h he la ice pa ame e o abou 3.60 Å. The la ice pa ame e o his Ni-like phase is sligh ly la ge han he one o pu e nickel (3.55 Å), hus indica ing alloying wi h la ge W a oms 20 40 60 80 100 120 140 0 4000 8000 12000 16000 measu ed da a Rie eld i di e ence W-B2 peak posi ions NiCo2W peak posi ions in ensi y (neu on coun / 1805 s) 2Θ (°) sample W_B measu ed a MEREDIT@NPL Figu e 1. Measu ed and calcula ed neu on di ac ion pa e n o W_B sample used o phase de e mina ion as well as o mic os ain cha ac e iza ion. The B agg posi ions o indi idual ecognized phases ( om he op W-B2 and NiCo2W; i should be no ed ha also he peak posi ions o λ /2 con amina ion wa eleng h a e shown) a e below he in ensi y cu e. The di e ence be ween he measu ed and calcula ed in ensi y is shown as well. Two phases we e iden i ied in all samples. The main phase is α -W (B2 s uc u e; wi hin he ex , i is e e ed o as W-B2 phase). The second phase wi h a weigh ac ion o 6%–7% has pu e-Ni-like s uc u e ( cc) wi h he la ice pa ame e o abou 3.60 Å. The la ice pa ame e o his Ni-like phase is sligh ly la ge han he one o pu e nickel (3.55 Å), hus indica ing alloying wi h la ge W a oms Ma e ials 2020,13, 208 4 o 15 (a omic adius o W, Ni and Co is 139, 124 and 125 pm, espec i ely). Du ing he s uc u al e inemen , i was assumed ha he second phase consis s o Ni and Co in he same a io as he ini ial composi ion (6:1) wi h a u he addi ion o 2 a .% o W. This seconda y phase is deno ed NiCo2W in wha ollows. I was ound using da a om 2D de ec o o TKSN-400 di ac ome e [ 28 ] ha he W_0 ba (i.e., he sample wi hou o a y swaging o ming) has a ine-g ained mic os uc u e o he W-B2 phase bu e y aw-g ained mic os uc u e o he NiCo2W phase. The NiCo2W phase p oduces spo s on he 2D de ec o while he W g ains o he W-B2 phase esul in a smoo h Debye–Sche e di ac ion conus, as can be seen in Figu e 2a. Taking in o accoun he gauge olume o 0.13 cm 3 , de ec o cha ac e is ics, and he geome ical a angemen o he expe imen , he g ain size o he NiCo2W phase in he W_0 sample can be es ima ed o be in he ange 0.2–1 mm. Ma e ials 2020, 13, x FOR PEER REVIEW 4 o 15 (a omic adius o W, Ni and Co is 139, 124 and 125 pm, espec i ely). Du ing he s uc u al e inemen , i was assumed ha he second phase consis s o Ni and Co in he same a io as he ini ial composi ion (6:1) wi h a u he addi ion o 2 a .% o W. This seconda y phase is deno ed NiCo2W in wha ollows. I was ound using da a om 2D de ec o o TKSN-400 di ac ome e [28] ha he W_0 ba (i.e., he sample wi hou o a y swaging o ming) has a ine-g ained mic os uc u e o he W-B2 phase bu e y aw-g ained mic os uc u e o he NiCo2W phase. The NiCo2W phase p oduces spo s on he 2D de ec o while he W g ains o he W-B2 phase esul in a smoo h Debye–Sche e di ac ion conus, as can be seen in Figu e 2a. Taking in o accoun he gauge olume o 0.13 cm3, de ec o cha ac e is ics, and he geome ical a angemen o he expe imen , he g ain size o he NiCo2W phase in he W_0 sample can be es ima ed o be in he ange 0.2–1 mm. (a) (b) Figu e 2. Pa o he di ac og am aken wi h 2D de ec o a TKSN-400 di ac ome e (in he angula ange 12.5–22°). (a) W_0 sample: Le s ip, W-B2 110 e lec ion; igh spo , NiCo2W 111 la ge-g ain e lec ion; (b) W_B sample: The smoo h s ips o in ensi ies om W-B2 110 (le ) and NiCo2W 111 ( igh ) e lec ions o ine-g ained phases a e o a y swaging. The la ge-g ain mic os uc u e is e ined by o a y swaging. W_A and W_B samples al eady exhibi he ine-g ained NiCo2W phase, as can be seen in Figu e 2b, aken o he same angula ange as Figu e 2a. The spo y pa e n o he NiCo2W phase changed he e o a smoo h pa e n o ine-g ained NiCo2W 111 e lec ion on he igh side o he angula ange while he cha ac e o he W-B2 110 e lec ion (on he le ) emained unchanged a e o a y swaging. The inding o he la ge-g ain mic os uc u e o he NiCo2W phase in he W_0 sample ba s essed he necessi y o o a e he samples a ound he e ical axis in o de o minimize he in luence o he la ge g ains on he esul ing di ac og am and consequen ly on he mic os ain de e mina ion. The esul s o neu on di ac ion analyses we e u he suppo ed ia elec on backsca e ing obse a ions. Figu e 3a,b shows EBSD scans depic ing he o ien a ions o he NiCo2W g ains in W_A and W_B samples, espec i ely. The depic ed colou s in he uni iangle indica e he o ien a ion o he axis no mal o he in es iga ed sample su ace in he c ys al e e ence ame. Wi h espec o he W_0 sample (no shown he e), he size o NiCo2W g ains was signi ican ly e ined and subs uc u e de eloped. The a e age NiCo2W g ain sizes we e 1.35 µm o he W_A sample and 1.0 µm o he W_B sample. Rega ding he W-B2 g ains, he o iginal W powde agglome a ed du ing sin e ing and o med pa icles wi h he sizes o se e al dozens o mic ome es, as can be seen in Figu e 3 and as was also epo ed p e iously [6]. I comes om he concu en ex u e in es iga ion by neu on sca e ing, which will be published elsewhe e, ha he e was no p e e en ial o ien a ion o he NiCo2W phase in he W_0 ba . On he o he hand, he NiCo2W phase was ex u ed wi h <111> c ys allog aphic di ec ions p e e en ially o ien ed along he sample ba axis a e o a y swaging. The ex u e was signi ican ly s onge o he cold swaged sample W_A han o he wa m swaged sample (W_B). The e is a Figu e 2. Pa o he di ac og am aken wi h 2D de ec o a TKSN-400 di ac ome e (in he angula ange 12.5–22 ◦ ). ( a ) W_0 sample: Le s ip, W-B2 110 e lec ion; igh spo , NiCo2W 111 la ge-g ain e lec ion; ( b ) W_B sample: The smoo h s ips o in ensi ies om W-B2 110 (le ) and NiCo2W 111 ( igh ) e lec ions o ine-g ained phases a e o a y swaging. The la ge-g ain mic os uc u e is e ined by o a y swaging. W_A and W_B samples al eady exhibi he ine-g ained NiCo2W phase, as can be seen in Figu e 2b, aken o he same angula ange as Figu e 2a. The spo y pa e n o he NiCo2W phase changed he e o a smoo h pa e n o ine-g ained NiCo2W 111 e lec ion on he igh side o he angula ange while he cha ac e o he W-B2 110 e lec ion (on he le ) emained unchanged a e o a y swaging. The inding o he la ge-g ain mic os uc u e o he NiCo2W phase in he W_0 sample ba s essed he necessi y o o a e he samples a ound he e ical axis in o de o minimize he in luence o he la ge g ains on he esul ing di ac og am and consequen ly on he mic os ain de e mina ion. The esul s o neu on di ac ion analyses we e u he suppo ed ia elec on backsca e ing obse a ions. Figu e 3a,b shows EBSD scans depic ing he o ien a ions o he NiCo2W g ains in W_A and W_B samples, espec i ely. The depic ed colou s in he uni iangle indica e he o ien a ion o he axis no mal o he in es iga ed sample su ace in he c ys al e e ence ame. Wi h espec o he W_0 sample (no shown he e), he size o NiCo2W g ains was signi ican ly e ined and subs uc u e de eloped. The a e age NiCo2W g ain sizes we e 1.35 µ m o he W_A sample and 1.0 µ m o he W_B sample. Rega ding he W-B2 g ains, he o iginal W powde agglome a ed du ing sin e ing and o med pa icles wi h he sizes o se e al dozens o mic ome es, as can be seen in Figu e 3and as was also epo ed p e iously [6]. I comes om he concu en ex u e in es iga ion by neu on sca e ing, which will be published elsewhe e, ha he e was no p e e en ial o ien a ion o he NiCo2W phase in he W_0 ba . On he o he hand, he NiCo2W phase was ex u ed wi h <111>c ys allog aphic di ec ions p e e en ially o ien ed along he sample ba axis a e o a y swaging. The ex u e was signi ican ly s onge o he cold swaged sample W_A han o he wa m swaged sample (W_B). The e is a ce ain ela ionship Ma e ials 2020,13, 208 5 o 15 be ween he ex u e and mechanical p ope ies. Ne e heless, he ela ionship is no desc ibed he e pu posely, as i will be a opic o a de ailed s udy published in a u u e pape . Ma e ials 2020, 13, x FOR PEER REVIEW 5 o 15 ce ain ela ionship be ween he ex u e and mechanical p ope ies. Ne e heless, he ela ionship is no desc ibed he e pu posely, as i will be a opic o a de ailed s udy published in a u u e pape . (a) (b) Figu e 3. Elec on backsca e di ac ion (EBSD) scan o he su ace pe pendicula o he sample-ba axis depic ing NiCo2W phase o sample: (a) W_A; (b) W_B. The depic ed colo s in he uni iangle indica e he o ien a ion o he axis no mal o he in es iga ed sample su ace in he c ys al e e ence ame. The g ay a eas a e W-B2 agglome a es. 3.2. Da a o Mic os ain De e mina ion Figu e 4a–c display he zoomed selec ed angula ange o he measu ed and calcula ed di ac og ams o all h ee samples wi h indexed e lec ions o bo h W-B2 and NiCo2W phases. In o de o display he ex en o sample peak b oadening, Figu e 4d addi ionally shows W_B sample da a oge he wi h a pa e n calcula ed wi hou any sample b oadening e ec . (a) (b) (c) (d) Figu e 4. De ail o measu ed and calcula ed di ac og ams showing he same indexed e lec ions om bo h W-B2 and NiCo2W phases in (a) W_0, (b) W_A and (c) W_B samples. (d) Addi ional W_B 68 72 76 80 84 88 0 5000 10000 15000 20000 25000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a Rie eld i in ensi y (neu on coun / 2222 s) 2Θ (°) sample W_0 measu ed a MEREDIT@NPL 68 72 76 80 84 88 0 4000 8000 12000 16000 20000 24000 28000 32000 36000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a Rie eld i in ensi y (neu on coun / 3600 s) 2Θ (°) sample W_A measu ed a MEREDIT@NPL 68 72 76 80 84 88 0 4000 8000 12000 16000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a Rie eld i in ensi y (neu on coun / 1805 s) 2Θ (°) sample W_B measu ed a MEREDIT@NPL 68 72 76 80 84 88 0 4000 8000 12000 16000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a simula ion o no-mic os ain sample in ensi y (neu on coun / 1805 s) 2Θ (°) sample W_B measu ed a MEREDIT@NPL Figu e 3. Elec on backsca e di ac ion (EBSD) scan o he su ace pe pendicula o he sample-ba axis depic ing NiCo2W phase o sample: ( a ) W_A; ( b ) W_B. The depic ed colo s in he uni iangle indica e he o ien a ion o he axis no mal o he in es iga ed sample su ace in he c ys al e e ence ame. The g ay a eas a e W-B2 agglome a es. 3.2. Da a o Mic os ain De e mina ion Figu e 4a–c display he zoomed selec ed angula ange o he measu ed and calcula ed di ac og ams o all h ee samples wi h indexed e lec ions o bo h W-B2 and NiCo2W phases. In o de o display he ex en o sample peak b oadening, Figu e 4d addi ionally shows W_B sample da a oge he wi h a pa e n calcula ed wi hou any sample b oadening e ec . Ma e ials 2020, 13, x FOR PEER REVIEW 5 o 15 ce ain ela ionship be ween he ex u e and mechanical p ope ies. Ne e heless, he ela ionship is no desc ibed he e pu posely, as i will be a opic o a de ailed s udy published in a u u e pape . (a) (b) Figu e 3. Elec on backsca e di ac ion (EBSD) scan o he su ace pe pendicula o he sample-ba axis depic ing NiCo2W phase o sample: (a) W_A; (b) W_B. The depic ed colo s in he uni iangle indica e he o ien a ion o he axis no mal o he in es iga ed sample su ace in he c ys al e e ence ame. The g ay a eas a e W-B2 agglome a es. 3.2. Da a o Mic os ain De e mina ion Figu e 4a–c display he zoomed selec ed angula ange o he measu ed and calcula ed di ac og ams o all h ee samples wi h indexed e lec ions o bo h W-B2 and NiCo2W phases. In o de o display he ex en o sample peak b oadening, Figu e 4d addi ionally shows W_B sample da a oge he wi h a pa e n calcula ed wi hou any sample b oadening e ec . (a) (b) (c) (d) Figu e 4. De ail o measu ed and calcula ed di ac og ams showing he same indexed e lec ions om bo h W-B2 and NiCo2W phases in (a) W_0, (b) W_A and (c) W_B samples. (d) Addi ional W_B 68 72 76 80 84 88 0 5000 10000 15000 20000 25000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a Rie eld i in ensi y (neu on coun / 2222 s) 2Θ (°) sample W_0 measu ed a MEREDIT@NPL 68 72 76 80 84 88 0 4000 8000 12000 16000 20000 24000 28000 32000 36000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a Rie eld i in ensi y (neu on coun / 3600 s) 2Θ (°) sample W_A measu ed a MEREDIT@NPL 68 72 76 80 84 88 0 4000 8000 12000 16000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a Rie eld i in ensi y (neu on coun / 1805 s) 2Θ (°) sample W_B measu ed a MEREDIT@NPL 68 72 76 80 84 88 0 4000 8000 12000 16000 NiCo2W 311 W-B2 220 NiCo2W 220 W-B2 211 measu ed da a simula ion o no-mic os ain sample in ensi y (neu on coun / 1805 s) 2Θ (°) sample W_B measu ed a MEREDIT@NPL Figu e 4. De ail o measu ed and calcula ed di ac og ams showing he same indexed e lec ions om bo h W-B2 and NiCo2W phases in ( a ) W_0, ( b ) W_A and ( c ) W_B samples. ( d ) Addi ional W_B sample da a oge he wi h heo e ical simula ion o a sample p o ile wi hou any mic os ain p esen in he NiCo2W phase (i.e., only he ins umen al b oadening e ec is p esen ). Ma e ials 2020,13, 208 6 o 15 By compa ing he measu ed peaks (see Figu e 4) o he W-B2 phase o he sample wi hou de o ma ion and samples a e he RS p ocess, no signi ican changes a e ecognized. On he o he hand, NiCo2W e lec ions b oadened signi ican ly wi h espec o pu e ins umen al b oadening (see Figu e 4d). This indica es an inc ease in mic os ain and disloca ion densi y in NiCo2W phase while he W-B2 phase was no a ec ed signi ican ly. The mic os uc u al i o he measu ed da a is discussed in Sec ion 4. 3.3. Elec on Mic oscopy Figu e 5shows a TEM scan o he W_A sample aken in a loca ion nea he NiCo2W/W-B2 in e ace. The subs an ial p esence o disloca ions wi hin he NiCo2W ma ix was obse ed. Ma e ials 2020, 13, x FOR PEER REVIEW 6 o 15 sample da a oge he wi h heo e ical simula ion o a sample p o ile wi hou any mic os ain p esen in he NiCo2W phase (i.e., only he ins umen al b oadening e ec is p esen ). By compa ing he measu ed peaks (see Figu e 4) o he W-B2 phase o he sample wi hou de o ma ion and samples a e he RS p ocess, no signi ican changes a e ecognized. On he o he hand, NiCo2W e lec ions b oadened signi ican ly wi h espec o pu e ins umen al b oadening (see Figu e 4d). This indica es an inc ease in mic os ain and disloca ion densi y in NiCo2W phase while he W-B2 phase was no a ec ed signi ican ly. The mic os uc u al i o he measu ed da a is discussed in Sec ion 4. 3.3. Elec on Mic oscopy Figu e 5 shows a TEM scan o he W_A sample aken in a loca ion nea he NiCo2W/W-B2 in e ace. The subs an ial p esence o disloca ions wi hin he NiCo2W ma ix was obse ed. Figu e 5. T ansmission elec on mic oscope image o W_A sample NiCo2W phase. 3.4. Ma e ial P ope ies The s ess-s ain cu es o W_0, W_A, and W_B samples a e depic ed in Figu e 6. The sin e ed W_0 sample exhibi ed he lowes UTS o app oxima ely 860 MPa. On he o he hand, he sample ea u ed a ela i ely high maximum elonga ion o mo e han 18%. As a esul o he in ensi e imposed shea s ain, he s eng h inc eased subs an ially; howe e , plas ici y (maximum elonga ion) dec eased a e bo h swaging egimes. The o al s eng hening, i.e., UTS, was highe o he W_A sample, whe eas he W_B sample ea u ed highe plas ici y. The physical p ope ies measu ed ia ul asound a e depic ed in Table 1 ( he a e age alue om 5 independen measu emen s aken pe sample). Table 1. Physical p ope ies esul ing om ul asound measu emen s. Sample Young’s Modulus (GPa) Shea Modulus (GPa) Poisson’s Ra io (-) W_0 340 130 0.280 W_A 350 137 0.278 W_B 359 141 0.270 Figu e 5. T ansmission elec on mic oscope image o W_A sample NiCo2W phase. 3.4. Ma e ial P ope ies The s ess-s ain cu es o W_0, W_A, and W_B samples a e depic ed in Figu e 6. The sin e ed W_0 sample exhibi ed he lowes UTS o app oxima ely 860 MPa. On he o he hand, he sample ea u ed a ela i ely high maximum elonga ion o mo e han 18%. As a esul o he in ensi e imposed shea s ain, he s eng h inc eased subs an ially; howe e , plas ici y (maximum elonga ion) dec eased a e bo h swaging egimes. The o al s eng hening, i.e., UTS, was highe o he W_A sample, whe eas he W_B sample ea u ed highe plas ici y. Ma e ials 2020, 13, x FOR PEER REVIEW 7 o 15 Figu e 6. Expe imen al s ess-s ain cu es o W_0, W_A, and W_B samples. 4. Da a Analysis and Discussion De ailed analysis o he measu ed neu on di ac ion da a was ca ied ou wi h he in en ion o de e mine mic os ain, disloca ion ype and disloca ion densi y. Wi h he suppo o he da a ob ained by o he echniques, hese mic os uc u al pa ame e s a e ela ed o he de e mined mechanical p ope ies. 4.1. Mic os ain De e mina ion Fi s , a phenomenological app oach was used o de e mine mic os ain and he line in eg al b ea hs o all he measu ed e lec ions. FullP o so wa e [30] enables he i ing o a phenomenological model o peak b oadening caused by mic os uc u al ea u es, pa icula ly mic os ain and g ain size, p o ided ha he ins umen al b oadening is known ac oss he whole measu ed 2θ ange. The ins umen p o ile dependency on sca e ing angle was ob ained by measu ing and i ing he s anda d SiO2 powde sample in he iden ical ins umen se up. The p o ile unc ion pa ame e s we e ex ac ed and s o ed in he ins umen esolu ion ile and his ile was used du ing s uc u al and mic os uc u al ull-pa e n e inemen . Then, he FullP o e inemen esul s in he sample con ibu ion o he e lec ion b oadening. This sample b oadening o he di ac ion peaks is epo ed in he u he ex . The e lec ion p o iles o he ungs en g ains (W-B2 phase) in he W_0 sample exhibi ed no sample b oadening. The e o e, no measu able mic os ain is p esen o his phase in he sin e ed sample. The small b oadening o di ac ion peaks in he W-B2 phase a e o a y swaging was obse ed. As he W-B2 phase g ains we e su icien ly la ge, no g ain-size b oadening was p esen . The sample b oadening o he W-B2 peaks was hen sa is ac o ily i using iso opic mic os ain. The ou pu was he maximum (uppe limi ) s ain e [31] which in ac ep esen s he mic os ain as i is connec ed wi h he oo mean squa e s ain (RMSS, 〈 〉/) h ough a cons an scaling ac o , 〈 〉/ =2/π. The de e mined W-B2 phase uppe limi s ain o he W_A and W_B samples was eW_A = 12.4 × 10−4 and eW_B = 10.8 × 10−4, espec i ely. I can be seen ha he e is sligh ly highe mic os ain in he W_A sample han in he W_B sample. In he case o he NiCo2W phase, peak b oadening was al eady p esen in he W_0 sample. A e o a y swaging, he sample b oadening e ec s ill signi ican ly inc eased. Al hough RS p ocedu e e ined he NiCo2W g ains, hey s ill emained su icien ly la ge in he measu ed samples (see Figu e 3). The g ain-size b oadening was hus no expec ed. As he e lec ions om (200) amily we e isibly mo e b oadened, he aniso opic s ain b oadening using S ephens o malism [32,33] was used o de e mine he mic os ain con ibu ion. The i was success ully ca ied ou assuming only mic os ain b oadening (i.e., no size b oadening). Gaussian p o ile, as usually done o mic os ain b oadening, was used o sa is ac o ily desc ibe he sample b oadening e ec . The ou pu s om he e inemen using he aniso opic s ain b oadening a e alues o in eg al b ead h o he indi idual e lec ions o he NiCo2W phase in ecip ocal space, β* = (β cosθ)/λ, whe e β is he in eg al b ea h in 2θ scale, and also mic os ain alues o he measu ed di ac ion Figu e 6. Expe imen al s ess-s ain cu es o W_0, W_A, and W_B samples. The physical p ope ies measu ed ia ul asound a e depic ed in Table 1( he a e age alue om 5 independen measu emen s aken pe sample). Ma e ials 2020,13, 208 7 o 15 Table 1. Physical p ope ies esul ing om ul asound measu emen s. Sample Young’s Modulus (GPa) Shea Modulus (GPa) Poisson’s Ra io (-) W_0 340 130 0.280 W_A 350 137 0.278 W_B 359 141 0.270 4. Da a Analysis and Discussion De ailed analysis o he measu ed neu on di ac ion da a was ca ied ou wi h he in en ion o de e minemic os ain, disloca ion ype anddisloca iondensi y. Wi h he suppo o heda aob ained by o he echniques, hese mic os uc u al pa ame e s a e ela ed o he de e mined mechanical p ope ies. 4.1. Mic os ain De e mina ion Fi s , a phenomenological app oach was used o de e mine mic os ain and he line in eg al b ea hs o all he measu ed e lec ions. FullP o so wa e [ 30 ] enables he i ing o a phenomenological model o peak b oadening caused by mic os uc u al ea u es, pa icula ly mic os ain and g ain size, p o ided ha he ins umen al b oadening is known ac oss he whole measu ed 2 θ ange. The ins umen p o ile dependency on sca e ing angle was ob ained by measu ing and i ing he s anda d SiO 2 powde sample in he iden ical ins umen se up. The p o ile unc ion pa ame e s we e ex ac ed and s o ed in he ins umen esolu ion ile and his ile was used du ing s uc u al and mic os uc u al ull-pa e n e inemen . Then, he FullP o e inemen esul s in he sample con ibu ion o he e lec ion b oadening. This sample b oadening o he di ac ion peaks is epo ed in he u he ex . The e lec ion p o iles o he ungs en g ains (W-B2 phase) in he W_0 sample exhibi ed no sample b oadening. The e o e, no measu able mic os ain is p esen o his phase in he sin e ed sample. The small b oadening o di ac ion peaks in he W-B2 phase a e o a y swaging was obse ed. As he W-B2 phase g ains we e su icien ly la ge, no g ain-size b oadening was p esen . The sample b oadening o he W-B2 peaks was hen sa is ac o ily i using iso opic mic os ain. The ou pu was he maximum (uppe limi ) s ain e[ 31 ] which in ac ep esen s he mic os ain as i is connec ed wi h he oo mean squa e s ain (RMSS, hε2 0i1/2 ) h ough a cons an scaling ac o , hε2 0i1/2=√2/πe . The de e mined W-B2 phase uppe limi s ain o he W_A and W_B samples was e W_A =12.4 × 10 −4 and e W_B =10.8 × 10 −4 , espec i ely. I can be seen ha he e is sligh ly highe mic os ain in he W_A sample han in he W_B sample. In he case o he NiCo2W phase, peak b oadening was al eady p esen in he W_0 sample. A e o a y swaging, he sample b oadening e ec s ill signi ican ly inc eased. Al hough RS p ocedu e e ined he NiCo2W g ains, hey s ill emained su icien ly la ge in he measu ed samples (see Figu e 3). The g ain-size b oadening was hus no expec ed. As he e lec ions om (200) amily we e isibly mo e b oadened, he aniso opic s ain b oadening using S ephens o malism [ 32 , 33 ] was used o de e mine he mic os ain con ibu ion. The i was success ully ca ied ou assuming only mic os ain b oadening (i.e., no size b oadening). Gaussian p o ile, as usually done o mic os ain b oadening, was used o sa is ac o ily desc ibe he sample b oadening e ec . The ou pu s om he e inemen using he aniso opic s ain b oadening a e alues o in eg al b ead h o he indi idual e lec ions o he NiCo2W phase in ecip ocal space, β *=( β cos θ )/ λ , whe e β is he in eg al b ea h in 2 θ scale, and also mic os ain alues o he measu ed di ac ion peaks o he NiCo2W phase in all h ee samples. The sample in eg al b ead h β * o each NiCo2W e lec ion is plo ed as a unc ion o ecip ocal la ice spacing o he pa icula e lec ion d* in Figu e 7(classical Williamson-Hall plo [31]), o W_0 and W_B samples. Ma e ials 2020,13, 208 8 o 15 Ma e ials 2020, 13, x FOR PEER REVIEW 8 o 15 peaks o he NiCo2W phase in all h ee samples. The sample in eg al b ead h β* o each NiCo2W e lec ion is plo ed as a unc ion o ecip ocal la ice spacing o he pa icula e lec ion d* in Figu e 7 (classical Williamson-Hall plo [31]), o W_0 and W_B samples. Figu e 7. Williamson-Hall plo o in eg al b ead hs in ecip ocal space o W_0 and W_B samples shown wi h linea i s h ough he poin s. When conside ing only he s ain b oadening componen as men ioned abo e, he uppe limi s ain e is connec ed wi h he in eg al b ea h by he o mula β* = 2 ed*, i.e., i s a e age alue can be calcula ed om he slope o he linea dependence o β* on d* [31]. The linea i s h ough he poin s a e shown in Figu e 7. The de e mined a e age sample mic os ain o he indi idual W_0, W_A, and W_B samples is hen e NiCo_0 = 14.2 × 10 −4 , e NiCo_A = 44.2 × 10 −4 and e NiCo_B = 41.2 × 10 −4 , espec i ely. I can be seen ha he mic os ain in NiCo2W phase e y signi ican ly (app oxima ely 3 imes) inc eased a e o a y swaging. Fu he , he e is a sligh ly highe NiCo2W-phase mic os ain in he W_A sample han in he W_B sample. Mos p obably, swaging a he empe a u e o 900 °C (W_B sample) enabled a pa ial dynamic ec ys alliza ion o NiCo2W phase. The aniso opic cha ac e o he NiCo2W phase in eg al b ead hs, isible in he Williamson-Hall plo (Figu e 7), indica es ha mic os ain is caused by disloca ions. Fu he , he subs an ial p esence o disloca ions in he NiCo2W ma ix was con i med by TEM obse a ions (Figu e 5). The e o e, he da a (i.e., acqui ed in eg al b ea hs o he NiCo2W phase indi idual e lec ions) we e u he analyzed in o de o de e mine he ac i e slip sys ems and o es ima e he disloca ion densi y a e he he momechanical p ocessing. 4.2. Disloca ion and Slip Sys em Type The ac ha disloca ion line b oadening is usually aniso opic, i.e., depends on hkl e lec ion, is well known (see [34] and e e ences he ein). I is gi en by he aniso opic cha ac e s o he displacemen ields o disloca ions (line de ec s), which, mo eo e , a e di e en o di e en ypes o disloca ions and slip sys ems. Then, he aniso opy analysis can be in p inciple used o cha ac e ize he pa icula ypes o occu ing disloca ions and ac i a ed slip sys em [35]. The e o e, we es ed his possibili y also in he NiCo2W phase o he sin e ed and o a y swaged samples. The aniso opy is cha ac e ized by he disloca ion a e age con as ac o s , which can be calcula ed wi h help o he ANIZC p og am [36] o a ious ypes o disloca ions o gi en cha ac e s and slip sys em α and o all he measu ed hkl e lec ions. The calcula ions (i.e., de e mina ion o he a e age con as ac o o he possible ypes o disloca ions) we e pe o med o he measu ed NiCo2W e lec ions. To pe o m he calcula ions, elas ic cons an s o he ma e ial we e needed [37]. In o de o use as p ecise alues o he elas ic cons an s o he NiCo2W solid solu ion as possible, he assump ion o a linea combina ion o he indi idual elas ic cons an s o he o iginal cons i uen s, Figu e 7. Williamson-Hall plo o in eg al b ead hs in ecip ocal space o W_0 and W_B samples shown wi h linea i s h ough he poin s. When conside ing only he s ain b oadening componen as men ioned abo e, he uppe limi s ain eis connec ed wi h he in eg al b ea h by he o mula β *=2ed*, i.e., i s a e age alue can be calcula ed om he slope o he linea dependence o β * on d* [ 31 ]. The linea i s h ough he poin s a e shown in Figu e 7. The de e mined a e age sample mic os ain o he indi idual W_0, W_A, and W_B samples is hen eNiCo_0 =14.2 ×10−4,eNiCo_A =44.2 ×10−4and eNiCo_B =41.2 ×10−4, espec i ely. I can be seen ha he mic os ain in NiCo2W phase e y signi ican ly (app oxima ely 3 imes) inc eased a e o a y swaging. Fu he , he e is a sligh ly highe NiCo2W-phase mic os ain in he W_A sample han in he W_B sample. Mos p obably, swaging a he empe a u e o 900 ◦ C (W_B sample) enabled a pa ial dynamic ec ys alliza ion o NiCo2W phase. The aniso opic cha ac e o he NiCo2W phase in eg al b ead hs, isible in he Williamson-Hall plo (Figu e 7), indica es ha mic os ain is caused by disloca ions. Fu he , he subs an ial p esence o disloca ions in he NiCo2W ma ix was con i med by TEM obse a ions (Figu e 5). The e o e, he da a (i.e., acqui ed in eg al b ea hs o he NiCo2W phase indi idual e lec ions) we e u he analyzed in o de o de e mine he ac i e slip sys ems and o es ima e he disloca ion densi y a e he he momechanical p ocessing. 4.2. Disloca ion and Slip Sys em Type The ac ha disloca ion line b oadening is usually aniso opic, i.e., depends on hkl e lec ion, is well known (see [ 34 ] and e e ences he ein). I is gi en by he aniso opic cha ac e s o he displacemen ields o disloca ions (line de ec s), which, mo eo e , a e di e en o di e en ypes o disloca ions and slip sys ems. Then, he aniso opy analysis can be in p inciple used o cha ac e ize he pa icula ypes o occu ing disloca ions and ac i a ed slip sys em [ 35 ]. The e o e, we es ed his possibili y also in he NiCo2W phase o he sin e ed and o a y swaged samples. The aniso opy is cha ac e ized by he disloca ion a e age con as ac o s Cα−hkl , which can be calcula ed wi h help o he ANIZC p og am [ 36 ] o a ious ypes o disloca ions o gi en cha ac e s and slip sys em α and o all he measu ed hkl e lec ions. The calcula ions (i.e., de e mina ion o he a e age con as ac o o he possible ypes o disloca ions) we e pe o med o he measu ed NiCo2W e lec ions. To pe o m he calcula ions, elas ic cons an s o he ma e ial we e needed [ 37 ]. In o de o use as p ecise alues o he elas ic cons an s o he NiCo2W solid solu ion as possible, he assump ion o a linea combina ion o he indi idual elas ic cons an s o he o iginal cons i uen s, i.e., Ni and Co, p esen in he a io o 6:1, was made. The conside ed alues ound in he li e a u e we e he ollowing: nickel [ 38 ]—C 11 =256.5 GPa, C 12 =151.5 GPa, C 44 =123.9 GPa; β -cobal ( cc) [ 39 ]—C 11 Ma e ials 2020,13, 208 9 o 15 =239.8 GPa, C 12 =163.4 GPa, C 44 =133.4 GPa. Thei linea combina ions used o es ima e he elas ic cons an s o he alloy we e hen: C11 =246.9 GPa, C12 =156.1 GPa, C44 =125.5 GPa. A e calcula ion o he a e age con as ac o s Cα hkl , a modi ied Williamson-Hall plo [ 37 ], i.e., he dependence o β * on d*C 1/2 , can be d awn. The esul s o he W_0, W_A, and W_B samples a e depic ed in Figu e 8a–o. As can be seen, he bes esul (conce ning i ing he linea dependence) o he W_0 sample was acqui ed o sc ew disloca ions and <111>slip sys em (Figu e 8e; he co esponding modi ied Williamson-Hall plo is ma ked by a ed ame). All he o he es ed disloca ion ypes and slip sys ems we e a wo se. On he o he hand, he slip sys em o <111>{110} edge disloca ions i s he bes o he measu ed in eg al b ead hs o W_A and W_B samples (Figu e 8g,l, espec i ely, ma ked by a ed ame). Ne e heless, he edge disloca ions wi h <110>{111} slip sys em (Figu e 8 ,k), as well as he sc ew disloca ions wi h <110>slip sys em (Figu e 8i,n), exhibi ed e y good linea i s o he o a y swaged samples, oo. The wo emaining es ed disloca ion ypes and slip sys ems (sc ew disloca ions and <111>slip sys em, and edge disloca ions wi h <111>{211} slip sys em) did no exhibi a su icien ly good i o any o he in es iga ed samples. Ob iously, ce ain mic os ain was p esen wi hin he s uc u e o he NiCo2W phase al eady a e sin e ing and subsequen cooling. The disloca ions p oduced du ing he sin e ing/quenching p ocess we e p edominan ly o a sc ew ype wi h <111>slip sys em. A e o a y swaging (W_A and W_B samples), he mic os ain inc eased signi ican ly (~3 imes) and he de o ma ion mechanism changed ei he o edge disloca ions wi h <111>{110} o <110>{111} slip sys em ( he la e occu s ypically in cc s uc u es [40]), o o sc ew disloca ions wi h <110>slip sys em. Ma e ials 2020, 13, x FOR PEER REVIEW 9 o 15 i.e., Ni and Co, p esen in he a io o 6:1, was made. The conside ed alues ound in he li e a u e we e he ollowing: nickel [38]—C 11 = 256.5 GPa, C 12 = 151.5 GPa, C 44 = 123.9 GPa; β-cobal ( cc) [39]—C 11 = 239.8 GPa, C 12 = 163.4 GPa, C 44 = 133.4 GPa. Thei linea combina ions used o es ima e he elas ic cons an s o he alloy we e hen: C 11 = 246.9 GPa, C 12 = 156.1 GPa, C 44 = 125.5 GPa. A e calcula ion o he a e age con as ac o s        , a modi ied Williamson-Hall plo [37], i.e., he dependence o β* on d*C 1/2 , can be d awn. The esul s o he W_0, W_A, and W_B samples a e depic ed in Figu e 8a–o. As can be seen, he bes esul (conce ning i ing he linea dependence) o he W_0 sample was acqui ed o sc ew disloca ions and <111> slip sys em (Figu e 8e; he co esponding modi ied Williamson-Hall plo is ma ked by a ed ame). All he o he es ed disloca ion ypes and slip sys ems we e a wo se. On he o he hand, he slip sys em o <111> {110} edge disloca ions i s he bes o he measu ed in eg al b ead hs o W_A and W_B samples (Figu e 8g,l, espec i ely, ma ked by a ed ame). Ne e heless, he edge disloca ions wi h <110> {111} slip sys em (Figu e 8 ,k), as well as he sc ew disloca ions wi h <110> slip sys em (Figu e 8i,n), exhibi ed e y good linea i s o he o a y swaged samples, oo. The wo emaining es ed disloca ion ypes and slip sys ems (sc ew disloca ions and <111> slip sys em, and edge disloca ions wi h <111> {211} slip sys em) did no exhibi a su icien ly good i o any o he in es iga ed samples. Ob iously, ce ain mic os ain was p esen wi hin he s uc u e o he NiCo2W phase al eady a e sin e ing and subsequen cooling. The disloca ions p oduced du ing he sin e ing/quenching p ocess we e p edominan ly o a sc ew ype wi h <111> slip sys em. A e o a y swaging (W_A and W_B samples), he mic os ain inc eased signi ican ly (~3 imes) and he de o ma ion mechanism changed ei he o edge disloca ions wi h <111> {110} o <110> {111} slip sys em ( he la e occu s ypically in cc s uc u es [40]), o o sc ew disloca ions wi h <110> slip sys em. (a) ( ) (k) (b) (g) (l) Figu e 8. Con .