Obtaining of combined titanium-steel structures by electron beam freeform fabrication using niobium and copper interlayers

doi:10.21203/rs.3.rs-3975628/v1

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Obtaining of combined titanium-steel structures by electron beam freeform fabrication using niobium and copper interlayers

https://doi.org/10.21203/rs.3.rs-3975628/v1

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published 11 Apr, 2024

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The work is devoted to the study of bimetallic structures "titanium-steel" by electron beam freeform fabrication with the use of niobium and copper interlayers. A metallographic study of the deposited interlayers is carried out. The hardness distribution over the samples is shown. Technological issues according to deposition of niobium on titanium and steel on copper are pointed out. Tensile testing results reveal that the obtained structures have an ultimate tensile strength of 150–228 MPa and the fracture is located at the niobium-copper alloy side or at the niobium interlayer. The need to reduce the titanium content in niobium due to the occurrence of intergranular penetration of copper is demonstrated.

combined construction

titanium-steel

electron-beam freeform fabrication

deposition

interlayer

intergranular penetration

niobium

copper

Nowadays, composite structures made of different materials are widely used to combine the properties of different materials in one construction or to reduce the consumbtion of expensive materials. Combined steel-titanium structures are of great interest. They combine the high corrosion resistance and low density of titanium with the high strength and workability of steel.

The main problem in obtaining the combined structure is the metallurgical incompatibility of titanium and iron. When this metal pair interacts, brittle intermetallides form and cause the destruction of the joint [1, 2]. Therefore, solid-state welding methods such as explosion welding [3, 4] and diffusion welding [5, 6], as well as fusion welding with the use of interlayers, are used to produce combined titanium-steel structures. Explosion welding is the most common method applied to obtain steel-titanium bimetallic plates. Despite the fact that this method does not involve melting, the products have localized melting in the area of the wave-like zones, which leads to embrittlement and cracking [4]. In the case of cylindrical products welding even more heating may occur which cause melting. This is due to the difficulties in the outflow of the gaseous explosion products [7]. It also should be noted that the use of both explosion and diffusion welding limits the geometry of the welded parts and reduces the repair manufacturability.

The use of free form fabrication by means electron beam makes it possible to obtain structures with any geometric configuration of the joint. It`s implementation makes it possible to increase the installation and repair work manufacturability. Refractory metals such as vanadium [8–14], niobium [15–23] and tantalum [10, 15, 24, 25] can be used for deposition on titanium alloy during additive forming. However, the use of tantalum may cause technological problems due to the large difference in melting temperatures. Vanadium and niobium are close to titanium in terms of metallurgical compatibility. Both metals are stabilisers of the titanium β-phase. Anyway, the formation of metastable α', α'' and ω phases is possible when the critical concentration in titanium is reached. However, according to scientific papers [12, 13, 33, 34], the formation of unfavourable ω-phase is revealed only in the Ti-V system. In the Ti-Nb system the formation of ω-phase is not observed [15, 16–23]. In addition to the formation of ω-phase, the creation of the unmixed region with zones of high and low titanium content is an important feature of the Ti-V system [14]. At the same time, the titanium enriched zones fulfil the conditions for the formation of the ω-phase. Taking into account the terms of the titanium interaction with refractory metals, the use of a niobium interlayer is preferable.

Considering that niobium is not metallurgically compatible with iron, it is essential to use the second interlayer, namely nickel [17, 26–31], copper [2, 6, 8, 9, 16, 19, 21–23] or alloys based on them. Based on the analysis of the nickel interaction with vanadium [26, 27, 28] and niobium [17, 29–31] the formation of brittle phases is noted in both systems [26, 29–31]. Hardness varies from 723 [31] to 2450 HV [26]. The strength properties of the construction are also not high and the relative elongation of the specimens does not exceed 2% [17, 30, 31]. Unlike nickel, copper does not form brittle compounds with neither refractory metals nor iron. Also, it is highly important that the melting point of copper is relatively low. It cause minimal melting of the substrate.

The use of two interlayers of niobium and copper to obtain combined structures is described in papers devoted to solid-phase welding [16] and fusion welding [16, 19–22]. At the same time, the possibility of obtaining such structures under the conditions of additive forming is insufficiently studied. The purpose of this study is to investigate the formation of bimetallic structures "titanium-steel" obtained by wire additive technologies through interlayers of niobium and copper.

Combined steel-titanium structures were fabricated by electron beam free form fabrication (EBFFF). Process of the combined structure production is presented on the Fig. 1. For this purpose, niobium wire Nb1 was deposited on a plate of titanium alloy VT1-0 with a size of 100x40x4. To reduce the concentration of titanium in the niobium interlayer, at least 3 beads of niobium were deposited on each sample. Then, at least 3 layers of copper were deposited on the top of the niobium interlayer by M0b copper wire. Low carbon steel wire Sv-08G2S was deposited after the copper interlayer as well. Before deposition of copper on niobium and mild steel on copper, the previous layer was milled. The number of deposited beads is given in Table 1. The electron beam deposition process was carried out on an electron beam system with an ELA-40I power supply with an accelerating voltage of 60 kV, equipped with a numerically controlled filler wire feed mechanism. The pressure in the vacuum chamber was 10^− 3 Pa.

Table 1

Number of deposited beads
Specimens №	Nb	Cu	Steel
1	5	3	5
2	4	3	-
3	5	-	-
4	6	3	-
5	7	3	-

The chemical composition of the applied materials is given in Table 2.

Table 2

Chemical composition of materials
Material	Chemical element, % wt.
VT1-0	Fe		C	Si		N		Ti		O		H		Total impurity
VT1-0	≤ 0.25		≤ 0.07	≤ 0.1		≤ 0.04		99.24–99.7		≤ 0.2		≤ 0.01		0.3
Nb-1	Nb	Fe			C		Si		N		H		O		Ta
Nb-1	Base	≤ 0,005			≤ 0,01		≤ 0,005		≤ 0.01		≤ 0.001		≤ 0.01		≤ 0.1
M0b	Fe		Ni	O		S		P		Pb		Zn		Cu + Ag
M0b	≤ 0,004		≤ 0,002	≤ 0,001		≤ 0,003		≤ 0,002		≤ 0,003		≤ 0,003		99,97
Sv-08G2S	C	Si			Mn		Ni		S		P		Cr		N
Sv-08G2S	0.05–0.11	0.7–0.95			1.8–2.1		≤ 0.25		≤ 0.025		≤ 0.03		≤ 0.2		≤ 0.01
St3sp	0,14 − 0,22	0,15 − 0,3			0,4 − 0,65		≤ 0,3		≤ 0,05		≤ 0,04		≤ 0,3		≤ 0,3

The electron beam deposition modes are shown in Table 3. The main adjustable parameters were wire feed speed w, deposition speed V, beam current I, sweep shape, sweep amplitude A and sweep frequency f. The beam current was chosen based on the need for proper substrate wetting with minimum penetration.

Table 3

Deposition modes
Wire feed rate, w (m/min)	Deposition speed, V (mm/min)	Beam current, I (mA)	Beam oscillation shape	Beam oscillation amplitude, А_х/A_y, (mm)	Beam oscillation frequency, f (Hz)
Deposition of niobium on titanium
0,6 − 0,85	125	11–16	circle	1,6/-	5
0,6 − 0,85	125	11–16	zigzag	1,5/1,7	10
Deposition of copper on niobium
0,15 − 0,2	125	9–14	zigzag	1,8/1,8	10
Deposition of low carbon steel on copper
0,3	125	8–12	zigzag	1/1,3	10

Three samples (№3, №4, №5) were fabricated to evaluate the mechanical properties of the combined structure. Before welding, the samples were milled to obtain flat edges. Sample №3, with a deposited niobium layer, was welded to St3sp steel using a M0b copper filler wire. The assembly for welding provided a gap of 2 mm and the copper substrate underneath. Four flat tensile specimens were cut after welding: two at the beginning (№3.1, №3.2) and two at the end (№3.3, №3.4). In the case of samples №4 and №5, the copper layer was deposited on the top of the niobium layer and then welded with St3sp steel. Four flat tensile specimens (4.1, 5.1–5.3) were prepared from these samples. Table 4 contains the selected welding modes.

Table 4

Welding modes
Specimen №	Welding speed, (mm/min)	Beam current, (mA)	Beam oscillation shape	Beam oscillation amplitude, А, (mm)	Beam oscillation frequency, f (Hz)	Tensile specimens №
3	250	25	circle	1.1	500	3.1–3.4
4, 5	1000	40	circle	0.75	100	4.1 5.1–5.3

In order to study the microstructure and hardness of the obtained combined structures, samples were prepared according to the following procedure: samples were cut on the AbrasiMatic 300 abrasive cutting machine, pressed on the SimpliMet 1000 hot pressing machine in phenolic-based compound, grinded on the EcoMet 250 grinding and polishing machine on carbide-silicon paper with grit P80-P2500 and polished with polishing cloths and suspensions of different dispersions. The microstructure was revealed by step by step chemical etching from the layer with the lowest chemical resistance to the layer with the highest one. The compositions of the used etchants are given in Table 5.

Table 5

The chemical composition of the applied etchants
Etchant №	Material	Compositions of the etchants
1	Titanium alloy	HNO₃:HF:H₂O = 2:1:10
2	Niobium	HNO₃:H₂O = 1:1
3	Copper	FeCl₃:HCl:H₂O = 1:6:20
4	Low carbon steel	HNO₃:C₂H₅OH = 1:25

Microstructural studies were carried out using Zeiss Observer Z1m optical microscope and Tescan MIRA 3 LMU scanning electron microscope. The chemical composition was measured using the EDS method on scanning electron microscope.

Hardness was indicated using Wolpert Wilson Instruments Vickers Hardness Tester 432SVD with a load of 1 kgf. In the fusion zones, the microhardness distribution was investigated at a load of 0.01 kgf. Wilson Hardness Tukon 2500 hardness tester was applied to determine the microhardness.

Flat tensile specimens from samples №4 and №5 were ground on the front and back of the weld to obtain a constant thickness of the workpiece. The tensile specimen from the sample №3 had the weld reinforcement. Tensile tests were performed on INSTRON 5982 electromechanical testing machine.

Figure 2 presents samples №3 and №4 after deposition of interlayers and welding with a steel plate.

Deposition of niobium on titanium

Fig. 3a depicts a panoramic view of the sample №1 after deposition of the niobium layer. Due to the large difference in melting temperatures, the titanium substrate melts significantly. As a result, the deposited beads have a different chemical composition, which is indirectly confirmed by their various degree of etchability. The results of the chemical analysis (Fig. 3b) indicate that the titanium content varies from 54.61% in the first bead to <0.5% in the 5th bead, and this distribution has a step-like character. The locations of the chemical composition measurements are marked by red squares in Fig. 3a.

In the first bead, where the titanium content is about 55%, a cellular-dendritic structure can be observed. On the elemental distribution map, the light areas correspond to crystals with an increased niobium content while the dark areas to a high titanium content, which liquefies along the crystallite boundaries (Fig. 4a). Vortices of different chemical composition, characterized by different etchability, are observed close to the fusion line with titanium (Fig. 4b). The formation of “vortices” is associated with hydrodynamic processes of metal transfer and incomplete mixing of the deposited material within high temperature gradient.

Fig. 5a shows the formation of a light interlayer of variable width near the fusion line. This interlayer is characterized by resistance to etching with etchant №2 (Table 5). After etching with etchant №1 (Fig. 5b), a needle structure of the martensitic type is observed.

For sample №1, the hardness peak of 222 HV1 was observed in the transition area (Fig. 6). This indicator does not exceed 275 HV0.01.

Equiaxed polygonal grains of 100-200 µm in size contain in the microstructure of the second bead, where the titanium content is approximately 17%. The intragrain structure is also represented by cellular or cellular-dendritic crystallites (Fig. 7a). From the third bead, the titanium content is less than 2%. The structure is particularly coarse grained with equiaxed grains exceeding 1 mm in size (Fig. 7b). No intragranular segregation is observed.

Deposition of copper on niobium

Due to the large melting temperature difference, niobium substrate melting is minimal or even absent. After deposition, the copper has a coarse-grained structure (Fig. 8) because of high-purity copper. The size of the particular grains reaches 3 mm.

According to the results of the chemical analysis, an abrupt change in chemical composition is noticed at the fusion line (Fig. 9a). As shown in Fig. 9b, zones of variable composition with a width of less than 1 μm were detected along the fusion line.

In sample №2 (Table 1) with a titanium content in the upper niobium bead of about 5-6%, intergranular penetration of copper is observed (Fig. 10). The maximum depth of penetration is 0.6 mm. The fourth bead in this sample was milled before copper deposition.

In sample №1, the titanium content in the upper niobium bead did not exceed 0.5% due to the deposition of five niobium beads. No intergranular penetration of copper along the fusion line was noted. It should be highlighted that liquid copper could flow down from the side of the deposited layer as a result of overheating due to the high thermal conductivity of the copper (Fig. 11a). Thus, for a short period of time when the copper was in the liquid state, intergranular penetration of copper (Fig. 11b) occurred in the second niobium bead across the entire width of the sample. An average titanium content in the zone of intergranular penetration was 17.8% (Table 6).

In the penetration region, several areas of different chemical composition can be identified (Fig. 12a, Table 6). It is noted that the titanium content in the penetration region exceeds the titanium content in the surrounding niobium grains.

Table 6

Chemical composition of different regions formed by copper penetration into the niobium interlayer

Location №	Element, % wt.
Location №	Nb	Cu	Ti	Si	O
1	2,04	71,44	25,75	0,05	0,72
2	0,60	81,59	17,10	0,11	0,60
3	77,99	0,70	17,94	0,14	3,22
4	79,28	0,42	17,61	0,14	2,55

It was not possible to reliably determine the microhardness in the penetration area due to its small width, the diagonals of the indents were larger than the dimensions of this area. However, an increase in hardness in the penetration area (Fig 12b) is evident based on the obtained results.

The hardness distribution in the copper layer is stable. The hardness of the copper layer is in the order of 50 HV1 (Fig. 13). There is a sharp change in hardness at the copper-niobium interface.

Deposition of low carbon steel on copper

Fig. 14a shows a panoramic view of sample №1 after low carbon steel deposition on copper.

Most of the copper melts mixes with the steel. The degree of copper melting varies in different sections of the sample and in some cases the steel penetrates to the niobium interlayer. The copper content in the deposited steel varies over a wide range. In the first bead, the copper content is approximately 42% wt., while in the fifth bead, the copper content decreases to 0.29% wt. The distribution of copper content in the deposited steel layer is shown in Fig. 14b. The structure of the first bead, which contains 41.5% Cu, is a mechanical mixture of copper and iron based solid solutions (Fig. 15a,b). Also due to the decrease in solubility of copper in iron during cooling, the formation of secondary and tertiary copper is observed in the first bead (Fig.15c). The second bead is represented by quenched structures with multiple inclusions of copper-based solid solutions of oval shape 1-3 µm in size (Fig. 15d). The copper content in the second bead is around 13%. The formation of a copper-based solid solution interlayer is notied at the fusion line of the first and second beads (Fig. 15b). Starting from the third bead, the amount of structurally free copper decreases. In the fifth bead, no structurally free copper is detected and the structure corresponds to the quenched one (Fig. 17). The hardness distribution is shown in Fig.16.

Tensile test results

Fig. 18 presents the results of the tensile tests.

The tensile strength of specimens №3.1, №3.2 and №3.4 is 219, 211 and 228 MPa, respectively. The stress-strain curve of the specimen №3.4 has an uncommon end section, which normally corresponds to the area of concentrated deformation. Analysis of the specimen (Fig. 19b) showed that the fracture occurred in an unusual manner: approximately half of the specimen cross-section fractured along the copper interlayer, while the other fractured past along the niobium interlayer. The fracture of specimens №3.1, №3.2 and №3.3 occurred along the copper-niobium fusion zone (Figure 19c). The worst results were obtained from specimen 3.3, apparently due to the presence of a welding defect in the copper-niobium fusion zone.

The melting of the steel and niobium interlayers can be seen in Fig.19a, 20, resulting in the formation of different structures in the copper matrix throughout the volume of the weld. The formation of the mechanical mixture of copper and steel is localized in a narrow area close to the steel interlayer.

Specimens №4.1, №5.1-№5.3 with a deposited copper interlayer have a lower tensile strength. The maximum value of the ultimate tensile strength is 170 MPa. However, the fracture of specimens №4.1, №5.1, №5.2 occurred along the niobium interlayer. A high ductility of the obtained specimens is also noted. Investigation of the fractured specimens showed that the reduction in area is 85-90%. The specimen 5.3 fractured along the fusion line of niobium and copper (Fig. 21c). Its tensile strength is 148 MPa. Fig. 21 presents panoramic views of specimens 4.1, 5.2 and 5.3 after fracture. It should also be noted that in specimens №5.1 and №5.3 there was intergranular penetration of copper, but none of these specimens fractured in the area of penetration.

Significant melting of the titanium substrate during deposition can be explaned by the different melting temperatures of niobium and titanium. This is the reason of a rather high concentration of titanium in the lower beads of niobium. In the fusion zone of titanium and niobium, where the formation of quenched structures is observed, the titanium content exceeds 95% by weight. The untypical shape of the interlayer in the fusion zone is associated with significant melting of the titanium substrate during the deposition process. In addition, the molten part of titanium crystallized after the crystallization of the first niobium bead. In this case, the liquid titanium was not able to mix with the deposited niobium, but a certain amount of niobium dissolved in it. As a result, quenched structures such as α' or α'' were formed in this zone. The increased hardness in the fusion zone indicated the formation of martensite α' or α''.

It should be noted that the formation of a quenched structures on the fusion line between niobium and titanium is not a significant problem as these structures have satisfactory ductility. However, uncontrolled melting of the titanium substrate is undesirable for several reasons. Firstly, excessive titanium content in niobium can lead to the formation of a zone with a β-stabiliser in titanium of a critical concentration. Exceeding this critical concentration can lead to the formation of the ω-phase and considerable embrittlement of the metal. Secondly, the increased concentration of titanium in niobium contributes to the activation of copper intergranular penetration (Figs. 10a,11b,12), which can cause a reduction in mechanical properties and fracture along the copper penetration areas. Therefore, it is necessary to minimise the melting of the titanium substrate. However, it is technically difficult to avoid melting at such big difference in melting temperatures. Thus, it is required to increase the number of deposited niobium beads.

Intergranular penetration of copper occurs in causes when titanium content in niobium was in the range of 15–20% wt. In the area of intergranular penetration, the formation of different structures was observed. On the basis of the chemical analysis data (Table 6, Fig. 12a) and phase diagram [35], it can be assumed that the eutectic Ti₂Cu₃ + β-TiCu₄ may be formed when there is 25.8 wt.%, while 17.10% wt. of titanium corresponded to the occurrence of β-TiCu₄.

Based on the fact that the niobium grain contains about 17.5% titanium, and in the area of intergranular penetration 25.8%, it can be proposed that titanium has a great ability to diffuse to grain boundaries. The formation of intermetallides in zones of copper penetration can cause a reduction in mechanical properties and a risk of compound fracture at grain boundaries weakened by brittle phases. The situation becomes more complicated by the great rate of copper penetration. Considering that the welding was done by an electron beam and that the intergranular penetration occurred after a drop of copper on the side surface, the copper was in a liquid state just for a short time. However, this was sufficient for penetration and for the formation of a copper net over the entire width of the niobium interlayer. It is also worth noting that intergranular penetration was observed in the top niobium bead at 5–6% wt. titanium content, but the depth of penetration was much less. There was no copper founded when the titanium content was less than 0.5% wt. It follows that the deposited niobium interlayer must have a titanium content of less than 0.5% wt. in the bead connected with a copper interlayer to form a defect-free structure.

The difference between melting point of steel and copper is significant. This results in melting and a significant amount of mixing of the copper interlayer with the deposited low carbon steel. In some cases, steel penetrates to the niobium interlayer. The copper content in the deposited beads varies over a wide range from 42 wt% to 0.3 wt%. The structure of the lower bead is a mechanical mixture of solid solutions based on copper and iron with a hardness of about 250 HV. In the following beads, the amount of copper decreases, which leads to the formation of a structure based on a solid solution of copper in iron. However, the release of excess copper is observed due to the low solubility of the elements in each other. The highest hardness is achieved in the second bead of the deposited low carbon steel. This is described by solid solution hardening of iron by copper, formation of quenched structures, dispersion hardening of steel by copper and phase hardening due to the large difference in linear expansion coefficients of copper and steel. In the following beads the hardness stabilises at 200–250 HV, while in the last bead there is a tendency to the hardness growth, which can be explained by the formation of hardening structures that have not been thermally affected by the deposition of the following beads (Fig. 17).

Tensile tests of specimens №3.1–3.4 obtained by welding with copper filler wire showed the mechanical properties at the level of pure copper. However, it should be noted that in most cases the fracture occurred in the zone of the copper-niobium alloy. This structure is represented by copper grains with inclusion of niobium dendrites. It seems that in the area of mechanical mixture of the niobium and copper phases, which have a large difference in linear expansion coefficients, great internal stresses are formed, leading to a fracture in this zone

In specimens №4.1, №5.1–5.3 the ultimate tensile strength corresponds to the level of pure niobium, and failure occurred almost always in niobium. The obtained difference in strength characteristics of samples №3 and №4, №5 can be explained by the constraint effect of the soft interlayer [36, 37, 38, 39]. Thus, a niobium interlayer with a low titanium content can be considered as the soft interlayer. In sample №3, the weld reinforcement was not removed, which caused swelling of the niobium interlayer. Therefore, the relative thickness of the low-titanium niobium layer was sufficiently small and conditions for the constraint effect were created. In samples №4 and №5, more niobium beads were deposited, and the weld reinforcement was removed so that the thickness of the soft niobium layer was too large for the constraint effect manifestation.

The comparison of the obtained mechanical properties in the papers [6, 21–23, 40] shows the similar values of tensile strength has. In the studies devoted to fusion welding [21–23, 40], the ultimate tensile strength ranges from 64 MPa [22] to 230 MPa [21]. In the most cases, the tensile strength of combined steel-titanium structures with the use of niobium and copper interlayers does not exceed 150 MPa. It should also be noted that in these studies, welding through thin interlayers was performed, which resulted in partial or complete remelting of the metals in combined structures. This lead to the formation of a brittle intermetallic phase and low ductility of the structures. In [22, 23, 40] the relative elongation do not exceed 2%. The additive forming process applied in this paper has a number of advantages over fusion welding. It makes it possible both to avoid the interaction of metallurgically incompatible materials and to obtain high ductility and strength properties at the level of the weakest interlayer. At the same time, it should be noted that it is possible to achieve similar results by using wider interlayers in fusion welding. The maximum strength properties were obtained by diffusion welding in the study [6]. The ultimate tensile strength of the structure was 300 MPa at -20°C and 270 MPa at 100°C, which is 20% higher than in this study. Fracture occurred along the fusion line between copper and niobium, copper and steel. Ductility values have not been reported. The thickness of the copper interlayer was 0.1 mm while the thickness of the niobium interlayer was 0.4 mm. The higher strength properties of the structure obtained by diffusion welding may be due to the constraint effect [36–39]. In this case, the main advantage of electron beam free-form fabrication is the possibility of obtaining a dissimilar structure with any joint shape and with comparable strength level and higher ductility compared to the considered works.

Tensile tests of combined titanium-steel structures with niobium and copper interlayers showed that the ultimate tensile strength of such a structure is 150–228 MPa, which is equivalent to the tensile strength of copper or niobium.

The deposition of niobium wire on titanium is technologically difficult due to the large difference in melting points. It requires the titanium substrate to be largely melted through to obtain a stable deposition mode. However, despite the structural heterogeneity of the first deposited bead, no defects were found, and the maximum hardness in the fusion zone did not exceed 275 HV0.01.

In the case of copper wire deposition on niobium, it is possible to achieve modes where the niobium does not melt. However, at high concentrations of titanium, around 17.5%, intergranular penetration of copper into the niobium interlayer is activated with possible formation of brittle phases at grain boundaries.

Deposition of steel wire on copper requires careful mode selection as the difference in melting points and the high thermal conductivity of copper can cause overheat of the copper interlayer and loss of stability of the bead formation till copper run-off. Copper in the deposited low carbon steel interlayer contributes to the hardening and dispersion hardening of the steel.

Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgments

The research was carried out with the financial support of the Russian Science Foundation (project No. 22-79-10338).

Data Availability

Data will be made available on request.

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Obtaining of combined titanium-steel structures by electron beam freeform fabrication using niobium and copper interlayers

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