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Investigation of the interface and physical properties of a Kovar alloy/Cu composite wire processed by multi-pass drawing

  • Jin-Hua Peng , Feng-Ze Pan , Ze-Xin Wang , Liang-Yu Chen , Cheng-Yu Pan , Dubovyy Oleksandr and Sheng Lu EMAIL logo
Published/Copyright: December 24, 2024
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High Temperature Materials and Processes
From the journal High Temperature Materials and Processes Volume 43 Issue 1

Abstract

A Kovar alloy composite wire inlaid with copper core was developed through hot isostatic pressing sintering and subsequent multi-pass drawing. The interface between the Kovar alloy and copper was revealed, and the physical properties of the composite wire were investigated. The results show that the Kovar alloy and copper diffuse mutually during the forming process, producing a stable metallurgical bond. When the diameter of the wire is 2.8 mm, a diffusion layer of about 16.5 μm was found at the interface. The concentration of the diffused element had a gradient distribution from the interface to both sides. Combining the excellent properties of Kovar alloy and copper, the composite wire has comprehensive physical properties. The electrical and thermal conductivities are 9.38 × 106 S·m−1 and 72.2 W·m−1·K−1, respectively. The composite wire has a low coefficient of thermal expansion, and the average coefficient of thermal expansion is lower than 6.36 × 10−6 ℃−1 in the temperature range of 25–450°C.

Keywords: Kovar alloy; copper; composite wire; physical properties

1 Introduction

With the development of the electric vacuum industry, the relationship between glass and metals has become particularly important. This puts forward higher requirements for sealing materials [1,2]. Thermal expansion is an important property for such sealing materials because glass has a low coefficient of thermal expansion. Within a certain temperature range, the sealing materials should have a coefficient of thermal expansion similar to that of glass, reaching a matched sealing [3]. Kavor alloy, made primarily of iron, nickel, and cobalt, is a common sealing material for glass and metals [4,5,6].

Kovar alloy has a high Curie point and excellent organizational stability at low temperatures. In the temperature range of 20–450°C, it shares a comparable coefficient of thermal expansion with hard glass [7,8,9,10]. Thus, Kavor alloy is suitable for sealing hard glass and has widespread application in high-vacuum glass–metal hermetic seals [11,12]. Recently, with the improvement in frequency and power of electron tubes, the sealing material should have high electrical conductivity and high thermal conductivity, as well as a low coefficient of thermal expansion [13,14,15]. Kovar alloy cannot meet these requirements due to its low electrical and thermal conductivity. Thus, it is important to enhance the electrical and thermal conductivities of Kovar alloy [16]. Considering the high electrical and thermal conductivity of copper, it is reasonable to produce Kovar alloy and copper composite and take advantage of their superior performance [17,18,19].

The aim of this study is to produce Kovar alloy and a copper composite wire and improve the electrical and thermal conductivities of Kovar alloy. The composite wire was produced by hot isostatic pressing (HIP) sintering and subsequent multi-pass drawing. The morphology and element distribution at the interface between Kovar alloy and copper were determined. The coefficient of thermal expansion and electrical and thermal conductivities of the composite wire were measured and discussed.

2 Experimental procedures

The materials used in this study are 4J29 Kovar alloy and pure copper. The 4J29 Kovar alloy has a chemical composition of 17% Co, 29% Ni, and the balance Fe. The original Kovar alloy rods have a diameter of 44 mm. A hole with a diameter of 14 mm was machined at the center of Kovar alloy rods. Then, copper rods with a diameter of 13.9 mm were produced and fitted into the hole. After that, the Kovar alloy and copper composite were subjected to HIP sintering. During HIP sintering, the temperature, pressure, and holding time were 1,000°C, 180 MPa, and 3 h, respectively. After HIP sintering, a multi-pass drawing was conducted on the composite at room temperature. For each pass drawing, the drawing deformation was about 15%. Since the composite wire experienced severe working hardening during cold drawing, before the next drawing, the composite was annealed at 900°C for 1 h to release the work hardening. After multi-pass drawing, composite wires with different diameters were obtained. In this study, the composite wires with diameters of 9.3 and 2.8 mm were analyzed.

The morphologies of the composite wire were observed using an optical microscope (OM) and a scanning electron microscope (SEM) on a cross-section. Elemental distribution at the interface was revealed by facial and linear SEM-EDS. A four-probe resistivity tester was used to measure the electrical resistivity and conductivity of the composite wire along the drawing direction. A thermal constant analyzer was used to measure the thermal conductivity of the composite wire along the drawing direction. Finally, the coefficient of thermal expansion was also measured along the drawing direction using a thermal expansion analyzer.

3 Results and discussion

Figure 1a and b shows the macro-morphology of Kovar alloy and copper composite wires after multi-pass drawing. The diameters of composite wires are 9.3 and 2.8 mm, respectively. Clearly, after multi-pass drawing, no oxidation or cracks are found at the surface of composite wires. Figure 1c and d shows the OM microstructure of the composite wires on a cross-section. The center zone is copper and it is surrounded by the Kovar alloy. It is also seen that the interface between the Kovar alloy and copper is smooth, indicating a good combination. However, after magnification of the interface through SEM, some discontinuous minute holes are found at the interface for the 9.3 mm composite wire. Different thermal expansion properties of Kovar alloy and copper could be responsible for these holes. During drawing and annealing, a radial shrinkage stress is produced at the interface due to the high coefficient of thermal expansion of copper. A higher stress concentration will be achieved when the composite wire is larger. The stress concentration at the interface can promote the formation of minute holes. In contrast, for the 2.8 mm composite wire, no holes are found at the interface due to lower stress concentration. Thus, through multi-pass drawing and annealing, Kovar alloy and the copper composite wire can be obtained with a good combination.

Figure 1 (a) and (b) Macro and (c)–(f) micromorphology of (a), (c) and (e) 9.3 mm and (b), (d) and (f) 2.8 mm composite wires.
Figure 1

(a) and (b) Macro and (c)–(f) micromorphology of (a), (c) and (e) 9.3 mm and (b), (d) and (f) 2.8 mm composite wires.

In order to reveal the element distribution at the interface of the composite wire, SEM-EDS was conducted on the interface. Figure 2a and b shows the facial and linear element distribution of the 9.3 mm composite wire. Clearly, after HIP sintering and multi-pass drawing, element diffusion occurred between the Kovar alloy and copper. Fe and Ni elements were on the copper side, while Cu was found on the Kovar alloy side. However, from the linear element distribution, it was found that the width of the diffusion layer was only 3.75 μm. The concentration of each element decreased sharply at the interface. These results indicate an inadequate microdiffusion at the interface. With further drawing to 2.8 mm, as shown in Figure 2c and d, the interface between the Kovar alloy and copper became blurry. An obvious element diffusion was also found at the interface. The width of the diffusion layer is 16.5 μm, which is much larger than that in the 9.3 mm composite wire. The concentration of each element decreased gradually from one side to another, showing a gradient distribution. In addition, it can be found that the diffusion of Cu and Ni is more significant than that of Fe. The reason is the low solid solubility of Fe in Cu, so the diffusion rate of Fe is low during HIP sintering and multi-pass drawing. The diffusion depths of Cu and Ni are also higher than that of Fe. From the element distribution along the interface, the Kovar alloy and copper have a good metallurgical bonding for the 2.8 mm composite wire.

Figure 2 (a) and (c) Facial and (b) and (d) linear element distribution at the interface for (a) and (b) 9.3 mm and (c) and (d) 2.8 mm composite wires.
Figure 2

(a) and (c) Facial and (b) and (d) linear element distribution at the interface for (a) and (b) 9.3 mm and (c) and (d) 2.8 mm composite wires.

According to the Fe–Cu phase diagram, Fe has a high solubility in the Cu matrix at high temperatures. However, Fe has a low diffusion rate in the Cu matrix, and a high content of Fe is dissolved on the surface of the Cu matrix, so the diffusion depth of Fe in the Cu matrix is small. In contrast, Cu and Ni diffused evenly at the interface to form a good metallurgical bond in certain areas. During the multi-pass drawing and high-temperature annealing, the diffusion depth of each element was significantly improved at the interface. This indicated that the diffusion of each element was promoted by continuous thermal-mechanical coupling. During the drawing process, residual stress was generated at the interface between the Kovar alloy and copper due to their different deformation abilities. Such residual stress can promote the element diffusion between the Kovar alloy and copper during subsequent annealing. Thus, with multi-pass drawing and annealing, the width of the diffusion layer became wider gradually. As a result, a wider diffusion layer was found in the 2.8 mm composite wire.

Electrical conductivity is important for improving the power of electronic prototypes [20,21]. The standard electrical conductivities of pure copper and 4J29 Kovar alloy are 5.95 × 107 and 2.08 × 106 S·m−1 at room temperature, respectively. The electrical conductivity of pure copper is much higher than Kovar alloy. Since temperature has a significant effect on the electrical conductivity of metals, the electrical conductivities of copper and Kovar alloy at different temperatures are calculated using the following equation [22]:

(1) σ T = σ T 0 1 + α R ( T − T 0 )

In this equation, σ T is the electrical conductivity (S·m−1), σ T 0 is the electrical conductivity (S·m−1) at room temperature, α R is the temperature coefficient of resistivity (K−1), and T is the temperature (K). The calculated electrical conductivities of copper and Kovar alloy are shown in Figure 3a and b. With an increase in temperature, the electrical conductivity decreased gradually. At 400°C, the electrical conductivities of copper and Kovar alloy are 2.39 × 107 and 9.24 × 105 S·m−1, respectively. In addition, the average temperature coefficient of resistance was also calculated for the composite wire. In the temperature range of 25–400°C, the value is about 3.71 × 10−3 °C−1, which is between the value of Kovar alloy and copper.

Figure 3 Calculated electrical conductivities of (a) pure copper and (b) Kovar alloy and the experimental electrical conductivity of (c) the composite wire at different temperatures.
Figure 3

Calculated electrical conductivities of (a) pure copper and (b) Kovar alloy and the experimental electrical conductivity of (c) the composite wire at different temperatures.

The electrical conductivity of the composite wire was measured using a four-probe tester from room temperature to 400°C, as shown in Figure 3c. At room temperature, the electrical conductivity is 9.38 × 106 S·m−1. It is higher than Kovar alloy but lower than that of the pure copper. With an increase in temperature, the electrical conductivity also decreased gradually. However, the electrical conductivity of the composite wire is much higher than that of Kovar alloy at different temperatures, which is more than three times.

Thermal conductivity is also important for the thermal performance of electro-vacuum components. As shown in Figure 4, pure copper has a high thermal conductivity, and it is much higher than that of the Kovar alloy [23,24]. With increasing temperature, the thermal conductivity of copper decreased gradually, while it increased slightly for the Kovar alloy. The thermal conductivity of the composite wire was measured using a hot disk thermal constant analyzer (steady state method), as shown in Figure 4c. It has a small variation with an increase in temperature and distributes between 72 and 73 W·m−1·K−1. Such thermal conductivity is much lower than that of copper, but it is about three times of Kovar alloy. This means that the combination of copper can significantly improve the heat-conducting properties of the Kovar alloy.

Figure 4 Thermal conductivities (α) of (a) pure copper, (b) Kovar alloy, and (c) their composite wire at different temperatures.
Figure 4

Thermal conductivities (α) of (a) pure copper, (b) Kovar alloy, and (c) their composite wire at different temperatures.

Figure 5 shows the variation of the coefficient of thermal expansion (α) and linear expansion rate (dL/L0) from 25 to 800°C. Clearly, the coefficient of thermal expansion and linear expansion rate of copper increase linearly with an increase in temperature. In contrast, the linear expansion rate of the Kovar alloy has a low increase rate when the temperature is below 450°C, while it increases quickly at higher temperatures. Thus, the coefficient of thermal expansion decreases first and increases gradually with the increasing temperature. The coefficient of thermal expansion has a minimum value (5.17 × 10−6 ℃−1) at about 430°C. The reason is the negative expansion property of the Kovar alloy below the Curie point, so it has good dimensional stability in this temperature interval [25,26]. The coefficient of thermal expansion and linear expansion rate of the composite wire show a similar change trend as that of the Kovar alloy. The minimum coefficient of thermal expansion is found at 400°C, which is about 6.36 × 10−6 °C−1. It is slightly larger than the Kovar alloy due to the combination of copper. However, the thermal expansion property of the composite wire has characteristics similar to that of the Kovar alloy. It also has an anomalous thermal expansion effect below the Curie point (450°C).

Figure 5 Coefficients of thermal expansion (α) and linear expansion rates (dL/L 0) of (a) pure copper, (b) Kovar alloy, and (c) their composite wire at 25–800°C.
Figure 5

Coefficients of thermal expansion (α) and linear expansion rates (dL/L 0) of (a) pure copper, (b) Kovar alloy, and (c) their composite wire at 25–800°C.

4 Conclusions

In summary, Kovar alloy and copper composite wires were produced by HIP sintering and multi-pass drawing. The composite wire has a good metallurgical combination between Kovar alloy and copper when the diameter is 2.8 mm. Obvious element diffusion was found at the interface, resulting in a 16.5 μm diffusion layer. The composite wire has excellent physical properties. At room temperature, the electrical and thermal conductivities were 9.38 × 106 S·m−1 and 72.2 W·m−1·K−1, respectively, which is several times higher than that of Kovar alloy. The composite wire has an anomalous thermal expansion effect, similar to that of Kovar alloy. Its minimum coefficient of thermal expansion is slightly larger than that of Kovar alloy.

Acknowledgments

The authors would like to express their sincere gratitude to the Special Project of Introducing Foreign Talents of Jiangsu Province (BX2022030) for their support of this project.

  1. Funding information: This work was supported by the Special Project of Introducing Foreign Talents of Jiangsu Province under Grant BX2022030.

  2. Author contributions: Jin-Hua Peng: conceptualization, formal analysis, and writing – review and editing. Feng-Ze Pan: methodology, validation and formal analysis. Ze-Xin Wang: conceptualization and methodology. Liang-Yu Chen: conceptualization and formal analysis. Cheng-Yu Pan: methodology. Dubovyy Oleksandr: conceptualization, validation, and formal analysis. Sheng Lu: conceptualization, writing – review and editing, and supervision.

  3. Conflict of interest: The authors state no conflict of interest.

  4. Data availability statement: The data that support the findings of this study are available from the corresponding author, upon reasonable request.

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Received: 2024-04-07
Revised: 2024-05-11
Accepted: 2024-05-14
Published Online: 2024-12-24

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  81. Computational role of homogeneous–heterogeneous chemical reactions and a mixed convective ternary hybrid nanofluid in a vertical porous microchannel
  82. Thermal conductivity evaluation of magnetized non-Newtonian nanofluid and dusty particles with thermal radiation
https://doi.org/10.1515/htmp-2024-0024
Keywords for this article
Kovar alloy; copper; composite wire; physical properties
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