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%mbin@ri metalice disimilare ob]inute prin sudarea prin difuzie Dissimilar metallic junctions obtained by solid diffusion welding

technique
Dr. ing. Violeta Tsakiris, Prof. dr. fiz. Wilhelm Kappel, Dr. ing. Georgeta Alecu, drd. fiz. Diana Cirstea, drd. fiz. Lucia Leonat, Dr. ing. Gimi R^mbu Institutul Na]ional de Cercetare }i Dezvoltare pentru Inginerie Electric@ - Cercet@ri Avansate ICPE-CA (INCDIE ICPE-CA), Bucure}ti
E-mail: violeta.tsakiris@icpe-ca.ro Sunt prezentate rezultatele cercetrilor experimentale privind obinerea unor cuple metalice disimilare, cum ar fi CuFe/Al, Ni-Al i FeCoV-Cu-Ti, prin utilizarea tehnologiei de sudare prin difuzie n faz solid. Jonciunile obinute sunt caracterizate la interfa din punct de vedere al caracteristicilor microstructurale, mecanice i electrice. Prezena la interfa a unor compui intermetalici cum ar fi Al2Cu, Al3Ni2, Ti2Cu3, s-a evideniat prin microscopie electronic i difracie de raze X. Sunt de asemenea, prezentai parametrii optimi de sudare prin difuzie (temperatura, timp de meninere, presiune, atmosfer, modul de pregtire al suprafeelor de mbinat) i posibilitile de aplicare ale jonciunilor realizate n industriile electrotehnic i electric sau n domeniul stomatologic.

Rezumat

Abstract

The experimental research results on the obtaining of some metallic dissimilar couples such as Cu-Fe/Al, Ni-Al and FeCoV-Cu-Ti by using solid state diffusion welding technique are presented. The obtained junctions were characterized at the interface from the microstructural, mechanical and electrical characteristics point of view. The presence of intermetallic compounds such as Al2Cu, Al3Ni2 and Ti2Cu3 at the interface was evidenciated by using electronic microscopy and X-ray diffraction. The optimum solid diffusion welding parameters (temperature, maintaining time, pressure, atmosphere, surface preparation) and the possibilities of junctions application in the electro-technical and electrical industries or in the stomatology field are also, outlined.

Dezvoltarea de noi materiale cu caracteristici specifice a condus la cerine mari in ceea ce privete tehnologiile de fabricaie i prin urmare, a procedeelor de mbinare. Tehnologia sudrii prin difuzie lrgete domeniul procedeelor de mbinare datorit posibilitilor combinaiilor de materiale. Aceasta tehnologie este esenial cnd, din motive tehnologice sau datorit caracteristicilor de material, nu pot fi aplicate alte tehnologii competitive de mbinare. Sudura prin difuzie reprezint un proces prin care se obine o jonciune ntre dou materiale similare sau disimilare. Are loc n faz solid cu creterea temperaturii prin procese de difuzie ale materialelor de mbinat n zona de difuzie. Rezultatul este o zon de difuzie care definete rezistena jonciunii [1]. n prima etap a procesului de sudare prin difuzie, deformarea plastic a asperitilor de la suprafa are loc prin deformare plastic i fluaj. n a doua etap are loc difuzia atomilor de la limitele de gruni spre goluri, n timp ce, n etapa a treia, se produce difuzia atomic volumic ctre goluri. Procesul de sudare prin difuzie se consider ncheiat atunci cnd, n urma aplicrii unei presiuni i a unei temperaturi la o interfa, pentru o anumit perioad de timp, cavitile de la suprafeele materialelor de mbinat se nchid complet [2]. SUDURA , XXII - 1/2012

1. Introducere

The development of new materials with specific characteristics leads to high demands in terms of manufacturing technologies and therefore, of joining processes. Diffusion welding technology expands the area of joining processes through the possibilities to combine different materials. This technology is essential when, for technological reasons or because of material characteristics other competitive joining technologies can not be applied. Diffusion welding is a process for obtaining a junction between two similar or dissimilar materials. It occurs in a solid phase with increasing the temperature through diffusion processes of the combined materials in the diffusion area. The result is a diffusion zone that defines the junction resistance [1]. In the first stage of diffusion welding, plastic deformation of the surface roughness occurs by plastic deformation and creep. In the second stage diffusion of atoms occurs from grain boundaries toward voids, while in the third stage, atomic volume diffusion occurs toward voids. Diffusion welding process is considered complete when, after applying pressure and temperature at an interface for a certain period of time, the cavities of the surfaces of both materials close completely [2]. Theoretically, all metals can be joined by diffusion due to 29

1. Introduction

Din punct de vedere teoretic, toate metalele pot fi mbinate prin difuzie datorit deformabilitii lor plastice. Ca temperatur de mbinare se considera 0,5...0,9 din temperatura de topire a metalelor de mbinat [1]. Metalele sunt mai potrivite pentru sudarea prin difuzie dect ceramicile fragile sau materialele silicioase, datorit condutivitii i ductilitii lor, care asigur o deformare plastic local mai bun a stratului de la suprafa, n domeniul micro. Metalele Al si Cu au conductivitate termic i electric bune i prezint o buna capacitate de turnare i prelucrabilitate. n special, aceste metale au rezistena mare la coroziune. Din cauza acestor considerente, aceste metale au fost utilizate n industria chimic, alimentar, de automobile, electrotehnic, la sisteme ale echipamentelor cu gaz, precum i sub form de bare tubulare umplute i folii [3]. Autorii lucrrii [3] au cercetat realizarea cuplelor metalice de Al-Cu prin metoda sudrii prin difuzie i prin metoda sudrii prin friciune. n timpul procesului de sudare s-au format compuii intermetalici Al2Cu, AlCu, Al4Cu9 care au un efect important asupra proprietilor mecanice. Diagrama de echilibru fazic Fe-Cu conine o reacie peritectic n partea bogat n Fe, figura1 [4].

Figura 1. Diagrama de faz@ Fe-Cu [4] Figure 1. Equilibrium phase diagram of Fe-Cu [4] Pentru acest sistem, datorit unei linii lichidus plate, se ateapt s existe o nemiscibilitate a fazei lichide metastabile, n topiturile subrcite, fapt confirmat i experimental, [5, 6]. Aceste metale prezint o solubilitate foarte mic, fiind practic nemiscibile, fiecare metal cristaliznd ntr-o reea bine definit: CVC pentru Fe i CFC pentru Cu. Autorii lucrrilor [7] i [8], au studiat materialele compozite micro-laminate NiAl/Ni pentru aplicaii structurale de temperatur nalt i blindaje. Compozitele micro-laminate NiAl/Ni au fost fabricate prin mbinare prin difuzie, sintez de reacie i post-tratament termic a multistraturilor alternative de Ni/Al. Analiza termic diferenial a aratat faptul c reacia dintre Al si Ni ncepe cu nucleerea i creterea NiAl3 la interfaa Ni/Al, urmat de dezvoltarea prin difuzie a compuilor Ni2Al3 la interfaa Ni/NiAl3. Dup tratamentul termic cu presiune aplicat, produii de reacie s-au 30

their plastic deformability. As joining temperature is considered 0.5.0.9 of melting temperature of the bonding metals [1]. Metals are more suitable for diffusion welding than brittle ceramics or silicon materials, because of their conductivity and ductility, which provides better local plastic deformation of the surface layer in the micrometer range. Al and Cu have good electrical and thermal conductivity and good casting and processability capacity. In particular, these metals have high corrosion resistance. Because of these considerations, these metals have been used for chemicals, food industry, automotive and electro-technical industry, gas equipments systems but also as filled tubular bars and sheets [3]. Authors of paper [3] have investigated the realization of Al-Cu metallic junctions by diffusion welding method and friction welding method. During the welding process, Al 2 Cu, AlCu, Al 4 Cu 9 intermetallic compounds were formed, which have an important effect on the mechanical properties. Equilibrium phase diagram of Fe-Cu contains a peritectic reaction the Fe rich area, Figure 1, [4]. For this system because of a flat liquidus line, an immiscibility of the metastable liquid phase is expected in the cooled melts and this fact is confirmed experimentally [5, 6]. These metals have very low solubility, practically being immiscible, each metal crystallizing with a well defined network structure: CCV for Fe and FCC for Cu. The authors of [7] and [8] papers had studied the micro-laminated composites of NiAl / Ni for high temperature structural applications and armors. NiAl / Ni micro-laminated composites were produced by diffusion bonding, reaction synthesis and post-heat treatment of the alternative multilayers of Ni / Al. Differential thermal analysis showed that the reaction between Al and Ni starts with the NiAl3 nucleation and growth at the Ni/Al interface, followed by diffusion development of Ni2Al3 compounds at the Ni/NiAl3 interface. After heat treatment while applying pressure, the reaction products were transformed into NiAl and Ni3Al with better resistance at high temperature. The literature 9 - 12, contains data on obtaining junctions between Ti/Ti alloys and austenitic steels, showing the formation of the Fe2Ti, FeTi, Fe2Ti4O, c, l and TiC fragile intermetallic phases in the diffusion zone, due to limited solubility of Fe and Ti with temperature. The difference in thermal expansion coefficients between Ti and austenitic steel is responsible for junction residual tensions. For this reason it is recommended to use appropriate intermediate materials that could minimize the formation of brittle intermetallic compounds and would also lead to an increase in the resistance properties of diffusion welded junction. In this paper, research results of Cu-Fe, Cu-Al, Al-Ni-Cu-Ti and FeCoV dissimilar metallic components performed by using diffusion welding technique, with potential applications in the electro-technical/electrical industry and dentistry, are presented.

2. Experimental

In the experiments to achieve dissimilar metal junctions of Cu-Fe, Cu-Al, Al-Ni-Cu-Ti and FeCoV by diffusion welding, the following metals were selected [13, 14]: iron plates of ARMCO type, containing C below 0.02%; electrolytical Cu plates of 99.9% purity; SUDURA , XXII - 1/2012

transformat n NiAl i Ni3 Al cu rezistena mai mare la temperatur ridicat. n literatura de specialitate 9 - 12, exist date referitoare la obinerea jonciunilor dintre Ti/ aliaje de Ti i oeluri austenitice, raportandu-se formarea fazelor intermetalice fragile de tip Fe2Ti, FeTi, Fe2Ti4O, c, l i TiC n zona de difuzie, datorit solubilitii limitate a Fe i Ti n funcie de temperatur. Datorit diferenei dintre coeficienii de dilatare termic ai Ti i oelului austenitic, n zona de mbinare apar tensiuni reziduale. Din acest motiv, este indicat s se utilizeze materiale intermediare corespunztoare care ar putea minimiza formarea compuilor fragili intermetalici i n plus, ar conduce i la o cretere a proprietilor de rezisten a jonciunii sudate prin difuzie. n lucrarea de fa, sunt prezentate rezultatele cercetrilor pentru realizarea unor componente metalice disimilare CuFe, Cu-Al, Al-Ni i FeCoV-Cu-Ti, prin tehnica sudrii prin difuzie, cu posibile aplicaii n industria electro-tehnic /electric i stomatologic.

n vederea experimentrilor pentru realizarea jonciunilor metalice disimilare Cu-Fe, Cu-Al, Al-Ni i FeCoV-Cu-Ti, prin sudare prin difuzie, au fost selectate metalele [13, 14]: plcue de Fe tip ARMCO cu un coninut de C sub 0,02%; plcue de Cu electrolitic de puritate 99,9 %; plcue de Al (marca 6060) de puritate 98,724%; Mn=0,03%; Si=0,463%; Cr=0,011%; Cu=0,034%; Ti=0,012%; Fe = 0,219%; Zn=0,047%; Mg=0,46%. plcue de Ni electrolitic (marca 28102) de puritate 99,97%; C=0,005%; Cu=0,001%; P=0,0002%; S=0,0005%; Co=0,0003%; Fe= 0,003%; Pb=0,0001%; Zn=0,0005%. discuri din aliaj Fe-Co-V cu 48%Co i 2%V; folie de Cu (99,95%); Ti comercial pur. Plcile de Ni electrolitic au fost reduse prin laminare de la grosimea de 5 mm, la grosimea de 3,5 mm i apoi au fost supuse tratamentului termic de recoacere n atmosfer de NH3 cracat, pentru ndepartarea ecruisajului indus prin operaia de laminare. Dup tratamentul de recoacere, plcile de Ni au fost supuse procesului de curare i activare a suprafeelor de mbinat. Dimensiunile semifabricatelor supuse ncercarilor de mbinare au fost: pentru jonciunea Cu-Fe: Cu: (85 x 20 x 5) mm; Fe: (88 x 20 x 11 ) mm; pentru jonciunea Cu-Al: Cu: (58 x 20 x 5) mm; Al (60 x 30 x5 ) mm; pentru jonciunea Ni-Al: Ni: (39 x 33 x 0,5) mm; Al: (39 x 30 x 5 ) mm; pentru jonciunea FeCoV-Cu-Ti: Fe-48Co-2V (% gr.) de (f 5x11) mm; folie de cupru de 40 mm grosime i Ti (f 5x6) mm. nainte de a fi supuse procedelului de mbinare, suprafeele de sudare ale plcuelor metalice au fost activate superficial prin polizare i lefuire pe hrtie metalografic. Pentru realizarea jonciunilor Cu-Fe/Al i Ni-Al, suprafeele plane de mbinare, astfel curate, au fost aduse n contact intim prin presare la 200 kg f /cm2. Pentru realizarea jonciunilor FeCoV-Cu-Ti, suprafeele de mbinare ale pieselor cilindrice au fost, de asemenea, pregtite prin tehnici obinuite de lefuire i polisare. Ca material intermediar s-a folosit o folie de cupru, curat n prealabil cu aceton i uscat n aer. 2.1. Parametrii tehnologici de sudare prin difuzie Experimentrile de mbinare ale cuplelor metalice Cu-Fe, Cu-Al i Al-Ni au avut loc ntr-un cuptor tip SAFED cu band continu, n atmosfer de NH3 cracat. Probele au fost fixate pentru mbinare cu metalele mai grele i cu puncte de topire SUDURA , XXII - 1/2012

2. Experimentri

Al plates (6060 mark) of 98.724% purity%; Mn=0,03%; Si=0,463%; Cr=0,011%; Cu=0,034%; Ti=0,012%; Fe = 0,219%; Zn=0,047%; Mg=0,46%. electrolytical Ni plates (28102 mark) of purity 99.97%; C=0,005%; Cu=0,001%; P=0,0002%; S=0,0005%; Co=0,0003%; Fe= 0,003%; Pb=0,0001%; Zn=0,0005%. discs of Fe-Co-V alloys with 48% Co and 2% V; Cu foil (99.95%), commercial pure Ti. The thickness of the electrolytical Ni plates was reduced by rolling from 5 mm to 3.5 mm and then, the plates were subjected to an annealing treatment in cracked NH3 atmosphere for hardening removal which was induced by the rolling. After annealing treatment, Ni plates have undergone the process of cleaning and activation of the joining surfaces. The dimensions of the semifinished parts subjected to the welding tests were the followings: for Cu-Fe junction: Cu: (85 x 20 x 5) mm, Fe: (88 x 20 x 11) mm; for Cu-Al junction: Cu: (58 x 20 x 5) mm, Al (60 x 30 x 5) mm; for Ni-Al junction: Ni: (39 x 33 x 0.5) mm; Al: (39 x 30 x 5) mm; for FeCoV-Cu-Ti junction: Fe-48Co-2V (% wt.) of 5 mm in diameter and 11 mm length, copper foil of 40 m thickness and Ti of f 5mm and 6 mm length. Before joining, the welding surfaces of metallic plates were superficial activated by grinding and polishing with metallographic paper. To achieve Cu-Fe/Al and Ni-Al junctions, flat joining surfaces, already cleaned, were brought in intimate contact by pressing at 200 kg f/cm2. To achieve FeCoV-CuTi junctions, joining surfaces of the cylindrical parts were also prepared by grinding and polishing common techniques. As an intermediate material a copper foil was used, cleaned before with acetone and air dried. 2.1. Technological parameters for diffusion bonding Welding experiments of the Cu-Fe Cu-Al and Al-Ni metallic couples, took place in a continuous band furnace of SAFED type, in cracked NH3 atmosphere. In order to be welded, samples were arranged in such a way that the heavier metals having higher melting points were placed on top of the lighter metals with lower melting points (Fe plates on top of Cu plates, Cu and Ni plates on top of the Al plates) and then, they have been arranged in graphite trays and placed on the furnace band. Ti/Cu/FeCoV ensemble was kept in contact in a fixing device and placed in a tubular furnace. Diffusion bonding was done in Ar atmosphere at 900 o C and maintained at this temperature for 1.5 h. Diffusion welding parameters selection was made based on previous experiments 15. Technological parameters used for diffusion welding of CuFe, Cu-Al and Al-Ni metallic couples are presented in Table 1.

3. Results and discussions

3.1 Characterizations of the obtained junctions A very good bonding at interfaces was observed by visual examination of the welded metallic components. In Figure 2 - 5, the macrographic aspects of the Cu-Fe, Cu-Al, Ni-Al and FeCoV-Cu-Ti components obtained by diffusion welding are presented. 3.1.1 Junctions analysis by optical microscopy and X-ray diffraction Specimens were sampled from the Cu-Fe/Al, Ni-Al and FeCoVCu-Ti metallic couples obtained by solid state diffusion in order to examine the interfaces areas by optical microscopy 31

mai ridicate deasupra celor mai uoare i cu puncte de topire mai sczute (plcile de Fe deasupra celor de Cu, plcile de Cu i de Ni deasupra celor de Al) i au fost asezate pe banda cuptorului pe tvie de grafit. Ansamblul Ti/Cu/FeCoV a fost inut n contact ntr-un dispozitiv de fixare i introdus ntr-un cuptor tubular. Sudarea prin difuzie s-a realizat n atmosfer de Ar, la o temperatur de 900oC cu meninere pe palier timp de 1,5 ore. Selecia parametrilor de sudare prin difuzie s-a efectuat n baza experimentrilor anterioare [15]. Parametrii tehnologici utilizai pentru care s-a obinut mbinarea cuplelor metalice Cu-Fe, Cu-Al i Al-Ni sunt prezentai n tabelul 1.

by using an optical microscope of of Carrziess type, with Axiovision software, and to detect the presence of the intermetallic phases in the diffusion area by X-ray diffraction and electronic microscopy. The specimens for optical microscopy examination were embedded into resin and polished with metallographic abrasive paper of SiC with a degree of fineness of grains of 400, 600, 800 and 1000 m, and then polished on velvet support with Al2O3 solution of 0,3 m. In Figure 6-9, the microscopic aspects of the cross section of Cu-Fe, Cu-Al, Al-Ni-Cu-Ti and FeCoV specimens, in the bonding areas of the metallic materials, are presented at x 500 magnification.

Tabel 1. Parametrii tehnologici de ^mbinare a cuplelor metalice Cu-Fe/Al }i Al-Ni Table 1. Technological parameters used for diffusion bonding of Cu-Fe, Cu-Al and Al-Ni couplings

3. Rezultate i discuii

3.1 Caracterizarea jonciunilor realizate Prin examinarea vizual a componentelor metalice sudate,

In the case of the Cu-Fe couple, in which Cu and Fe are almost immiscible, Figure 1 [4], the welding at interface was done by diffusion processes and hot plastic deformation at micro level, by the interplay of the copper between the

Figura 2. Jonc]iuni Cu-Fe Figure 2. Cu-Fe Junctions

Figura 3. Jonc]iuni Cu-Al Figure 3. Cu-Al Junctions

Figura 4. Jonc]iuni Ni-Al Figure 4. Ni-Al Junctions s-a constatat o lipire foarte bun la interfee. n figurile 2- 5 sunt prezentate aspectele macrografice ale componentelor CuFe, Cu-Al, Ni-Al i FeCoV-Cu-Ti, obinute prin sudare prin difuzie. 32

Figura 5. Jonc]iuni FeCoV-Cu-Ti-Al Figure 5. FeCoV-Cu-Ti-Al harder asperities of the Fe, Figure 6. In the case of the Cu-Al and Al-Ni metallic couples, the optical microscopy images have shown the presence of a very SUDURA , XXII - 1/2012

Figura 6. Zona de interfa]@ Cu-Fe x 500 Figure 6. Cu-Fe interface area x 500

Figura 7. Zona de interfa]@ Cu-Al x 500 Figure 7. Cu-Al interface area x 500

Figura 8. Zona de interfa]@ Al-Ni x 500 Figure 8. Al-Ni interface area x 500 3.1.1 Analiza jonciunilor prin microscopie optic i difracie de raze X Din cuplele metalice Cu-Fe/Al, Ni-Al i FeCoV-Cu-Ti, realizate prin sudarea prin difuzie n faz solid, au fost prelevate probe n vederea examinrii zonelor de interfa, prin microscopie optic la un microscop optic de tip Carrziess cu soft Axiovision iar prezena fazelor intermetalice din zona de difuzie a fost investigat prin difracie de raze X i microscopie electronic. Probele supuse examinrii prin microscopie optic au fost nglobate n rin, prelucrate prin lefuire cu hrtie metalografic abraziv de SiC cu un grad de finee a granulaiei de 400, 600, 800 i 1000 m i apoi lustruite pe suport de catifea cu soluie de Al2O3 de 0,3 m. n figurile 6 i 9 sunt prezentate aspectele microscopice ale probelor Cu-Fe, Cu-Al, Al-Ni i FeCoV-Cu-Ti, n seciune transversal, n zonele de mbinare ale materialelor metalice, la mrire x 500. n cazul cuplului Cu-Fe, n care metalele Cu i Fe sunt aproape nemiscibile, figura 1 [4], sudarea la interfa s-a realizat prin procese de difuzie i de deformare plastic la cald, la nivel micro, prin ntreptrunderea cuprului ntre asperitile mai dure ale Fe, figura 6. n cazul cuplelor metalice Cu-Al i Al-Ni, imaginile de microscopie optic, au artat prezena unor zone foarte nguste de difuzie (@0,30,6 m), att la interfaa Cu-Al ct i la interfaa Ni-Al, figurile 7 i 8, n timp ce pentru cuplul FeCoV-Cu-Ti zona de difuzie este de aproximativ 47 m, figura 9. n figurile 10 i 11 (a i b) sunt prezentate imaginile de microscopie electronic la interfaa jonciunilor Cu-Al i NiAl efectuate la un microscop electronic de baleiaj cu fascicul SUDURA , XXII - 1/2012

Figura 9. Zona de interfa]@ FeCoV-Cu-Ti x 500 Figure 8. FeCoV-Cu-Ti interface area x 500 narrow diffusion area (@0,30,6 m), both at the Cu-Al interface and Ni-Al interface, Figure 7 and 8, while for the FeCoV-Cu-Ti couple the diffusion area is about 47 m, Figure 9. In the Figure 10 and 11 (a and b), the electron microscopy images of the Cu-Al and Ni-Al interface junctions performed with a scanning electron microscope with focused ion beam, FIB-FESEM, Auriga model, with imaging and elemental chemical quantification (EDS + SEM), and the quantitative analysis of analyzed spectra in the diffusion areas, are presented. The elemental analysis reveals that for the CuAl junction, the AlCu3 and Al2Cu + Cu intermetallic compounds type were formed in the diffusion area close to Cu side (Figure 10 a) and AlCu3 and Al2Cu + Al compounds in the diffusion area close to Al side (Figure 10 b). For the NiAl couple, compounds of Al3Ni2 + Ni type, and Al3Ni2 + Al respectively, were determined in the diffusion area close to Ni (Figure 11a) and in the area close to Al diffusion (Figure 11b), respectively. Intermetallic compounds in the diffusion area of the FeCoV/Cu/Ti ensemble obtained by diffusion welding have been highlighted by X-ray diffraction technique, Figure 12. At 900 C, the atomic activity over the joining surfaces is increasing causing a significant interdiffusion. At this temperature, besides Ti phase which has a hexagonal structure, the Ti2Cu3 (Cu4Ti3) intermetallic compounds with tetragonal structure and Cu3Ti intermetallic compound with orthorhombic structure were revealed. The X-ray images revealed the presence of compounds with tetragonal structure of Al2Cu type and of Al4Cu9 type with cubic structure for the Cu-Al metallic couples, which were 33

a
Figura 10. Imagini SEM la jonc]iunea Cu-Al ^n zona apropiat@ de Cu (a) }i de Al (b) Figure 10. SEM images at Cu-Al junction in the area near to Cu (a) and Al (b) concentrat de ioni, FESEM-FIB, model Auriga, cu imagistic i cuantificare elemental chimic (EDS + SEM) i analizele cantitative ale spectrelor analizate n zonele de difuzie. Din analiza elemental rezult c, la jonciunea Cu-Al, s-au format compui intermetalici de tip AlCu3 i Al2Cu + Cu, n zona de difuzie apropiat de Cu (figura 10a) i compui AlCu3 si Al2Cu + Al n zona de difuzie apropiat de Al (figura 10 b). n cazul cuplei Ni-Al, s-au determinat compui de tip Al 3 Ni 2 + Ni i respectiv, Al 3 Ni 2 + Al n zona de difuzie apropiat de Ni (figura 11a) i respectiv, n zona de difuzie apropiat de Al (figura11b). Compuii intermetalici din zona de difuzie a ansamblului FeCoV/Cu/Ti obinut prin sudare prin difuzie, au fost evideniai prin tehnica de difracie de raze X, figura 12. La 900 oC,

actually found also by the authors of [3], Figure 13 a) while for the Al-Ni metallic couple, the compounds with hexagonal structure of Al3Ni2 type, Figure 13 b) were determined. 3.1.2. Junction characterization from mechanical and electrical point of view From the realized metallic couples there were sampled specimens in order to their characterization at interface, in terms of mechanical properties (Vickers microhardness measurements) and electrical (resistivity and electrical conductivity measurements). Vickers microhardness measurements were performed with a microhardness tester of EM 700 type, with Precidur software and the resistivity and electrical conductivity tests were conducted by four points method, by using TESLA BM

Figura 11. Imagini SEM la jonc]iunea Ni-Al ^n zona apropiat@ de Ni (a) }i de Al (b) Figura 11. SEM images at Ni-Al junction in the area near to Ni (a) and Al (b) activitatea atomic de-a lungul suprafeelor de mbinare crete determinnd producerea unei interdifuzii semnificative. Pe lng faza de Ti care are o structur hexagonal, la aceast temperatur s-au pus n eviden compuii intermetalici Ti2Cu3 (Cu4Ti3) cu structur tetragonal i compusul intermetalic Cu3Ti cu structur ortorombic. Pentru cuplele metalice Cu-Al, imaginile de raze X au pus 34 395 bridge. In the Figure 14, 15 and 16, the graphs of variation of Vickers microhardness measured on the metallic matrix of Cu, Fe, Al and Ni and also, on the interfaces of the obtained metallic couples were presented. Variation curve of the Vickers microhardness values measured on the Cu matrix, on the Cu-Fe interface, and on SUDURA , XXII - 1/2012

Figura 12. Analiza prin difrac]ie de raze X a suprafe]ei de desprindere la jonc]iunea ansamblului FeCoV-Cu-Ti ^mbinat prin difuzie la: 900 oC/1,5 ore Figure 12. X-ray diffraction of a detachment surface coming from the FeCoVCu-Ti ensemble junction bonded by diffusion at: 900 oC/1,5 hrs

the Fe matrix, is shown in Figure14. From Figure 14 it is revealed that the micro-hardness value obtained on the Cu-Fe interface (108 HV0,1) shows an increase with 34 HV0,1 in compare with the average value recorded on the matrix (74 HV0,1) and a decrease with 33 HV0,1, in compare with the average value of microhardness obtained on the matrix of Fe (141 HV0,1). By micrographs examination of the Cu-Al diffusion welded samples (Figure 7) it is shown that there is a diffusion area of approx. 0.6 mm, and an area of intermetallic compounds in Al matrix. The existence of the hard compounds of Al2Cu type with tetragonal structure, and of Al4Cu9 type with cubic structure, at the bonding line of Cu-Al, Figure10 and13 a), increases the microhardness value (203 HV), Figure 15. By micrographs examination of the Ni-Al samples diffusion welded it is observed the existence of a diffusion area of approx. 0, 3 mm and of an intermetallic compound zone near to the Al matrix, Figure 8 . The existence of the hard compounds in the Ni-Al junction interface, with hexagonal structure of Al3Ni2 type, Figure 11 and

n eviden prezena compuilor cu structur tetragonal de tip Al2Cu i cu structur cubic a de tip Al4Cu9, fapt constatat i de autorii lucrrii [3], (figura13 a) iar pentru cuplele metalice AlNi, compui cu structur hexagonal, de tip Al3Ni2 (figura13 b). 3.1.2. Caracterizarea jonciunilor din punct de vedere mecanic i electric Din cuplele metalice realizate, au fost prelevate probe n vederea caracterizrii acestora la interfa, din punct de vedere al proprietilor mecanice (msurtori de microduritate Vickers) i electrice (msurtori de rezistivitate i conductivitate electric). Msurtorile de microduritate Vickers s-au efectuat, la un microdurimetru de tip EM 700, cu soft Precidur iar testele de rezistivitate i conductivitate electric s-au realizat, prin metoda celor patru puncte, cu ajutorul punii TESLA BM 395. n figurile 14, 15 i 16 sunt prezentate graficele de variaie ale microduritii Vickers msurate b att pe matricile metalice de Cu, Fe, Al i Ni ct i la interfeele cuplelor metalice obinute. de variaie a valorilor de microduritate Vickers, msurate pe matricea de Cu, la interfaa Cu-Fe i pe matricea de Fe, este prezentat n figura 14. Din figura 14 se constat c valoarea microduritii obinut la interfaa Cu-Fe (108 HV0,1) arat o cretere cu 34 HV0,1 fa de valoarea medie nregistrat pe matricea de Cu (74 HV0,1) i o diminuare cu 33 HV0,1, fa de valoarea medie a microduritii pe matricea de Fe (141 HV0,1). Din examinarea micrografiilor probelor Cu-Al sudate prin difuzie ( figura 7 ) se constat existena unei zone de difuzie de aproximativ 0,6 m i a unei zone de compui intermetalici n matricea de Al. Existena compuilor duri cu structura tetragonal, de tip Al2Cu i cu structura Figura 13. Difrac]ie de raze X la interfa]a Cu-Al (a) }i la interfa]a Ni-Al (b) cubic, de tip Al4Cu9, la linia de mbinare Cu-Al, Figure 13. X-ray diffraction at the Cu-Al interface (a) and at the Ni-Al interface (b) SUDURA , XXII - 1/2012 35

Metallic couples of the Cu-Fe, Cu-Al, Al-Ni and FeCoV-Cu-Ti respectively, can be achieved in a continuous band furnace, and a tubular furnace respectively, in a controlled at-mosphere, with proper preparation of the joining surfaces and ensuring of a mini-mum contact pressure. Optimal parameters that led to the obtaining of successful junctions of Fe, Cu, Ni and Al, and FeCoV, Cu and Ti respectively, dissimilar metals were the followings: w diffusion welding temperature: 1100 10 oC (Fe-Cu) 640-650 oC (Al-Cu) and 660670 o C (Al-Ni) 9505 o C (FeCoV-Cu-Ti); w band furnace speed: max. 180 oC (Cu-Fe and Al-Cu) mm/min, max. 90 oC (Al-Ni) mm/min; heating speed of 5 o C/min (FeCoV-Cu-Ti); w maintaining time on band: 102min (Cu-Fe), 82 min (Al-Cu), 162 min (Al-Ni); Figura 15. Valori ale microdurit@]ii Vickers (HV 0,025) ob]inute pe matricea de w working atmosphere: NH3 cracked for Cu la interfa]a }i matricea de Al Cu-Fe, Cu-Al and Al-Ni, and Ar atmosphere Figure 15. Vickers microhardness values (HV 0.025) performed on the Cu for FeCoV-Cu-Ti respectively. matrix, the Cu-Al interface and Al matrix By diffusion processes and local plastic mativ 0,3 m i a unei zone de compui intermetalici n deformation by creep, at micro level, there were obtained apropierea matricei de Al, figura 8. Existena compuilor successful and qualitative Cu-Fe, Cu-Al, Al-Ni, and FeCoVduri de la interfaa jonciunii Ni-Al, cu structur hexagonal Cu-Ti respectively, dissimilar metal junctions, as evidenced de tip Al3Ni2, figurile 11 i 13 b), confirm valorile mari ale by optical and electronic microscopy images. microduritii obinute (155 HV), figura 16. n tabelul 2 sunt prezentate msurtorile de rezistivitate (r) i conductivitate electric (s), pentru metalele de mbinare utilizate Fe, Cu, Al i Ni, precum i pentru cuplele metalice studiate Fe-Cu, Cu-Al i Ni-Al. Rezultatele obinute arat c valorile proprietilor electrice obinute pentru cuplele metalice realizate, se ncadreaz n intervalul de variaie al conductivitii electrice (105 i 108 W-1x cm-1) i al rezistivitii electrice (10-5 i 10-8 W x cm), specifice materiale metalice compacte [16]. figurile 10 i 13 a), determin creterea microduritii (203 HV), figura15. Din examinarea micrografiilor probelor Ni-Al sudate prin difuzie se constat existena unei zone de difuzie de aproxi-

Figura 14. Valori ale m@sur@torilor de microduritate efectuate pe matricea de Cu, la interfata Cu-Fe }i pe matricea de Fe Figure 14. Vickers microhardness measurements valuesperformed on the Cu matrix, the Cu-Fe interface and Fe matrix

13b) confirms the high values of the obtained microhardness (155 HV), Figure 16 . In Table 2, it is shown the measurements values of resistivity ( r ) and electrical conductivity (s), of the Fe, Cu, Al and Ni used bonding metals, and also those obtained on the Fe-Cu, Cu-Al and Ni-Al studied metallic couples. Results showed that the electrical properties values obtained for the realized metallic couplings are within the range of variation of the electrical conductivity (105 i 108 W-1x cm-1) and of the electrical resistivity (10-5 i 10-8 W x cm), which are specific to the compact metallic materials [16].

4. Conclusions

4. Concluzii

Cuplele metalice Cu-Fe, Cu-Al, Al-Ni i respectiv, FeCoV-Cu-Ti pot fi realizate n cuptor cu band continu i respectiv, n cuptor tubular n atmosfer controlat, n conditiile pregtirii corespunzatoare a suprafeelor de mbinare i asigurrii unei presiuni minime de contact. 36

Figura 16. Valori ale microdurit@]ii Vickers (HV 0,025) ob]inute pe matricea de Ni, zona de difuzie }i matricea de Al Figure 16. Vickers microhardness values (HV 0.025) obtained in the Ni matrix, the Ni-Al diffusion area and Al matrix. With the transition from Cu matrix to Fe matrix, the Vickers microhardness measurements showed intermediate values of microhardness obtained on the Cu-Fe interface (108 SUDURA , XXII - 1/2012

Parametrii optimi care au condus la obinerea unor Tabel 2. Valorile rezistivit@]ii }i conductivit@]ii electrice, pentru metalele mbinri reuite ale metalelor disimilare Fe, Cu, Ni i Fe, Cu, Al }i Ni, precum }i pentru cuplele metalice Cu-Fe, Cu-Al }i Ni-Al, ob]inute prin sudarea prin difuzie Al, respectiv FeCoV, Cu i Ti au fost: w temperatura de sudare prin difuzie: 110010 oC Table 2. Electrical resistivity and conductivity values for the Fe, Cu, Al and Ni metals, and Cu-Fe Cu-Al and Ni-Al metallic couplings, obtained (Fe-Cu) 640-650 oC (Al-Cu) i 660-670 oC (Al-Ni) 950 by diffusion welding 5 oC (FeCoV-Cu-Ti); w viteza band cuptor: max. 180 oC (Cu-Fe i Al-Cu) mm/min, max. 90 o C (Al-Ni) mm/min; viteza de nclzire de 5 oC/min (FeCoV-Cu-Ti); w timp de meninere pe band: 102 min (Cu-Fe), 82 min (Al-Cu), 16 2 min (Al-Ni); w atmosfer de lucru: MH3 cracat pentru Cu-Fe, CuAl i Al-Ni, i respectiv, atmosfer de Ar pentru FeCoVCu-Ti. n urma proceselor de difuzie i de deformare plastic local prin fluaj, la nivel micro, s-au obinut jonciuni metalice disimilare reuite i de calitate Cu-Fe, Cu-Al, Al-Ni i respectiv, FeCoV-Cu-Ti, fapt evideniat prin imaginile de microscopie optic i electronic. La tranziia dinspre matricea de Cu spre matricea de Fe, msurtorile de microduritate Vickers au demonstrat obi-nerea unor valori intermediare ale microduritii la interfaa Cu-Fe (108 HV0,1 ), comparativ cu cele obinute pe matricea de Cu (74 HV 0,1 ) i matricea de Fe (141 HV0,1). mbinarea metalelor disimilare Cu i Al se realizeaz ca HV0,1), in compared with those obtained on the Cu matrix urmare a proceselor de difuzie i fluaj, cu formare de (74 HV0,1) and matrix of Fe (141 HV0,1). compui intermetalici duri de tip Al2Cu i Al4Cu9, cu struc- Joining of Cu and Al dissimilar metals is achieved due to tura tetragonal, respectiv cubic. mbinarea metalelor Al diffusion and creep processes, with formation of tough cu Ni, are loc prin procese de difuzie i fluaj, cu formare de intermetallic compounds of Al2Cu and Al4Cu9 type having compui intermetalici de tip Al3Ni2, cu structura hexagonal. tetragonal structure, and cubic structure, respectively. The Formarea la interfat a compuilor intermetalici, determin bonding of Al and Ni metals occur by diffusion and creep creterea valorilor de duritate: 55 HV pentru Al-Ni i respectiv, processes, with formation of intermetallic compounds of 203 HV pentru Al-Cu. n cazul jonciunii FeCoV-Cu-Ti, prin Al3Ni2 type with hexagonal structure. difracie de raze X, s-a evideniat existena compuilor The formation of intermetallic compounds at interface inintermetalici Ti2Cu3 (Cu4Ti3) cu structura tetragonal i a creases the hardness values: 55 HV for Al-Ni and 203 HV for compusului Cu3Ti cu structura ortorombic. Al-Cu, respectively. In the case of the FeCoV-Cu-Ti junction, Jonciunile realizate Cu-Fe, Cu-Al i Al-Ni, au prezentat valori the X-ray diffraction has revealed the existence of the Ti2Cu3 ale proprietilor electrice, asemntoare materialelor (Cu4Ti3) intermetallic compounds with tetragonal structure compacte, metalice. and of Cu3Ti with orthorhombic structure. Cuplele metalice disimilare Cu-Fe mbinate prin difuzie n Junctions made of Cu-Fe, Cu-Al and Al-Ni had values of faz solid, pot fi utilizate pentru anumite aplicaii n indus- electrical properties, like compact metallic materials. tria electrotehnic (de exp. n condiiile existenei unor fore Cu-Fe dissimilar metallic couples bonded by solid phase electromotoare mari), n scopul reducerii consumului de diffusion can be used for certain applications in the electroCu i mbuntirii performanelor mecanice ale acestuia. technical industry (i.e. when there are large electromotive Cuplele metalice disimilare Cu-Al i Ni-Al pot fi utilizate forces), to reduce Cu consumption and to improve its pentru aplicaii n industria electrotehnic i/sau electric. mechanical performances. De exemplu, jonciunile metalice disimilare Cu-Al pot fi Cu-Al and Ni-Al dissimilar metallic couples can be used for folosite sub form de plci la bornele generatoarelor de la applications in the electro-technical and/or electrical turbine, cu partea din cupru n contact cu borna din cupru industry. For example, Cu-Al dissimilar metallic junctions a generatorului i cu partea din aluminiu n contact cu can be used as plates at the turbine generators terminals, conductorul din aluminiu. n acest fel, se asigur un contact with the copper in contact with the copper borne of the electric optim i tensiunile electromotoare de contact sunt generator and aluminum in contact with the aluminum diminuate. conductor. In this way, it provides an optimal electrical Din jonciunea particular FeCoV-Cu-Ti realizat din contact and the contact electro-motor tensions are reduced. materiale disimilare, s-a realizat un pivot de forma celui From the particular junction of FeCoV-Cu-Ti made of prezentat n figura 5, pentru a fi utilizat n stomatologie. dissimilar materials, it was made a pivot in the form of that Acest pivot mpreun cu un ataament dentar magnetic presented in Figure 5, to be used in dentistry. This pivot asigur fixarea protezei dentare, prin intermediul unei fore together with a magnetic dental attachment provides magnetice de atracie denture fixation via a magnetic force of attraction. Autorii mulumesc pentru suportul financiar acordat, prin Proiectul nr. 06-30-01-16/2008 i Proiectul nr. 229906/2009ICPE-HyFC. Acknowledgement The authors thank for the financial support granted by Project. No 06-30-01-16/2008 and Project. No 229906/2009ICPE-HyFC. 37

SUDURA , XXII - 1/2012

Bibliografie/References
[1] Dahmms St., Basier U., Khler G.: Diffusion welding An alternative joining procedure, chances and limitations for exemplary applications, South-East European Welding Congress, Timisoara, 2006, p. 203211. [2] Mahoney M. W., and Bampton C.C.: Fundamentals of Diffusion Bonding, ASM Handbook-Welding, brazing and soldering, vol 6, 1993. [3] Ifran AY, Sare CELIK, Ibrahim CELIK: Comparison of properties of friction and diffusion welded joints made between the pure aluminium and copper bars BAU Fen Bilimleri Enstitusu Dergisi,1999. [4] Massalschi T. B: Binary Alloy Phase Diagrams, ASM, Metals Park, OH, 1980. [5] Elder S. P., Abaschian G. S.: Proc. Principle of Solidification and Materials Processing, R. Trivedi, J. A. Sekhar, and J. Mazumdar, eds., Oxford and IBH Publishing Co Ltd., New Delhi, 1989, vol 1, p. 1-299. [6] Muniz A.: Metall. Trans. B, 1987, vol. 18B, p. 75-565. [7] Hee Y. Kim, Dong S. Chung, Soon H. Hong: Reaction synthesis and microstructures of NiAl/Ni micro laminated composites Materials Science and Engineering A 396, 2005, p. 376 384. [8] Morsi K.: Mater. Sci. Eng. A 299, 2001, p. 1-15. [9] Gosh M., Kundu S., Chatterjee S., and Mishura B., "Influence of Interface Microstructure on the Strength of the Transition Joint between Ti-6Al-4V and Stainless Steel," Metallurgical and Materials Transactions A, Vol. 36A, July 2005-1891. [10] Kundu S., Gosh M., Laik. A., Bhanumurthy K., Kale G. B., Chatterjee S.: Diffusion bonding of commercially pure titanium to 304 stainless steel using copper interlayer, Materials Science and engineering A 407, 2005, p. 54-160. [11] He P., Zhang J., Zhou R., Li X.: Diffusion bonding technology of a titanium alloy to a stainless steel web with an Ni interlayer. Materials Characterization, 1999, 43, 287-92. [12] Gosh M., Chatterjee S., Mishra B.: The effect of intermetallics on the strength properties of diffusion bonds formed between Ti-5.5Al-2.4V and 304 stainless steel, Materials Science and Engineering A 363, 2003, p. 268-274. [13] Tsakiris V.: mbinri de materiale printr-o tehnic special-sudur prin difuzie, Proiect PN 06-30-01-16/2007, Faza 2/15.11.2008. [14] Tsakiris V., Cristinel I., Marinescu V., Rosu R., Petica A., Popa M., Chirita I.: Pivots for magnetical fixing of dental prosthesis obtained by diffusion welding technique, The 4th International Conference 10-11.06.2010, Timisoara, Romania-Innovative technologies for joining advanced materials, p.266-271, Ed.SUDURA Publishing House ISSN 1844-4938. [15] Tsakiris V., Lucaci M., Sbrcea G., Marinescu V.: Characterization of diffusion welded joints between titanium and permendur type alloy using different interlayers 3rd International Conference Innovative Technologies For Advanced Materials, 11 -12.06.2009, Timioara, pag. 148-151 (CD), ISSN 1844-4938. [16] Ursache M., Chirc D.: Proprietile metalelor, Ed. Did. i Ped. Bucureti, 1982.

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