Experimental investigation on development and machinability of copper matrix hybrid composite – graphene and SiC / TiC / ZrO₂ / AlMg reinforcements

ABSTRACT

A copper – graphene base composite is developed with different hard particle reinforcements through the powder metallurgy process. The different reinforcement particles are silicon carbide (SiC), titanium carbide (TiC), zirconium oxide (ZrO2) and aluminum – magnesium (AlMg) at equal weight percentages. The spherical copper powder with irregular reinforcement particles got pressed during the powder compaction and deformed to form a strong structure. During sintering the powder compaction has undergone metallurgical diffusion and the bonding between the reinforcement and matrix material. The microstructure of the pure copper and the copper – graphene with different reinforcement is compared for discussion. The hardness of copper and copper – graphene – titanium carbide composite is maximum and similar in results. The density of copper – graphene – titanium carbide composite is two-fold harder than the copper – graphene – aluminum magnesium composite material. Subsequently the porosity of the AlMg reinforcement is less as the diffusivity is higher than the other reinforcements.

Keywords:
Copper; Graphene; Reinforcement; Density; Machinability

1. INTRODUCTION

Copper composites are in demand for many engineering applications such as frictional material, energy conducting material and domestic utensils. To improve the mechanical and physical properties of the copper composite, research is recommended to reinforce carbon base reinforcement along with the other reinforcement material [¹, ²]. The difficulty in handling the carbon base reinforcement in the base metal is agglomeration. For example, the liquid metallurgy process leads to unwanted reaction, reinforcement floating and repulsion during the casting process [³]. Powder compaction is one the best techniques to produce copper – carbon base composite for wide applications [⁴]. Sintering is the predominant factor to justify the quality of the powder compaction samples. Energy developed during the sintering process and the soaking time will induce the particles to diffuse and get metallurgical bonding of the material [⁵]. To improve the mechanical strength and structural properties of the copper base metal matrix composite, the borides, nitrides and carbides are the common reinforcement used as exceptional reinforcements [⁶, ⁷]. In addition to carbides and other compounds; literature on rare earth refractories and their reinforcement is available in the existing research. MOUSTAFA et al. [⁸] reported the copper matrix with silicon carbide and alumina as a reinforcement in the hybrid composite material developed through the powder metallurgy concept. It was claimed that the addition of hard particles will improve the material bulk properties in terms of strength and metallurgical aspects. In the same way the other reinforcements such as titanium carbide, zirconium oxide and aluminium – magnesium are also used in the copper base composite. LI et al. [⁹] reported that the development of TiC in the copper base composite is highly recommended as a tool for electrical discharge machining. In the presence of TiC in the composite has a drastic influence to improve the density and conductivity of the EDM tool. As part of the research, machining composite is one of the challenges in the machining process. The machinability includes recent advances in the machining processes such as abrasive water jet cutting, wire electrical discharge machining, laser cutting, electron beam machining and many more [¹⁰,¹¹,¹²,¹³]. A graphene and silicone composite gel has outstanding fire resistance, suggesting that it could be used to reduce coal seam fires [¹⁴]. A silver-graphene composite coating that is produced by varying the brush plating voltage and brush plating time exhibits a slightly lower self-corrosion potential and a lower self-corrosion current than a pure silver coating, suggesting that the composite coating has superior corrosion resistance [¹⁵]. Due to the improved dispersion and stronger interfacial bonding of GO inside the polycaprolactone (PCL) matrix, improvements in thermal stability and biocompatibility were observed. Therefore, adding graphene and graphene oxide (GO) to PCL nanocomposites greatly improves their characteristics, making them appropriate for demanding biological applications [¹⁶]. The novelty of the research is to develop the copper base composite with graphene and carbides / oxides through a powder metallurgy process. Composite is further post processed to enrich the mechanical and metallurgical properties through the sintering process. Results are evaluated following the industrial standard and it is validated. In continuation to the research, the wire electrical spark erosion method is used to machine the copper base matrix material with different reinforcement. From the investigation, the justifications and the recommendations are made.

2. MATERIALS AND METHODS

Copper base composite materials with different types of reinforcement are developed through the powder compaction method. The pure (99.9%) copper powder particle with 30 ± 5 µm is used as a source for base matrix material. Five different Cu base composites are developed with the particles such as silicon carbide (SiC); titanium carbide (TiC); zirconium oxide (ZrO²); aluminium – magnesium (AlMg) and graphene (Gr) are used as individual reinforcement materials. All the reinforcement particles are of the similar size and the particles are measured in the range of 30 ± 5 µm. The weight percentage of the copper (Cu) particle is the matrix material which is fixed as a 90%, the graphene (Gr) is 3% and the reinforcement is maintained as 7% for all the composites. The combination of matrix and the reinforcements are mechanically mixed using a ball milling machine to avoid the agglomeration and clusters of matrix and reinforcements. The ball milling machine operates at a speed of 250 revolutions per minute for 60 minutes continuously to blend the matrix and reinforcements. Considering the compact load aspect ratio, the length and diameter of the samples are maintained as 120 mm long and 12 mm in diameter. To reach out this sample dimension the metal powders are weighed. A carbon alloy steel die is used for green compaction with a hydraulic press at a defined constant pressure 700 ± 5 MPa as press load. The compacted samples are further sintered using a box furnace at a constant temperature of 800 ± 5°C for a soaking time of three hours.

Further the samples after sintering are investigated to justify the quality of the composites in terms of metallurgical and mechanical properties following ASTM standards. The microhardness of the composite (ASTM E92 – 2023), density (ASTM D 792 – 20) and porosity are measured to indicate the mechanical properties. On the other way, the machinability of the composite material is also investigated using wire electro spark machining process performed in Electronica BMG 830 machine. A 0.2 mm copper – zinc half hard wire material is used as an electrode and the deionized water is used as dielectric medium. The machining of Cu base composite materials is made with different pulse duration to study impact on surface roughness and its topography. Table 1 infer the detail on input process parameters used to machine copper base composite material. The Mitutoyo SJ210 surface roughness meter is used to measure the roughness value and the VEGA3 scanning electron microscope to reveal the surface topography of the machined surface. From the experimental result technical justifications are drawn and the composite is recommended for the future scope.

Table 1
Input process parameters used to machine copper base composite material.

PARAMETERS	RANGE	UNITS
Pulse on Time	110, 115 and 120	µs
Pulse off time	10 and 30	µs
Voltage	50	Volt
Wire tension	7	kg/mm
Duty factor	90	%
Cutting speed	1	mm/min
Electrolyte	Deionized water

3. RESULTS AND DISCUSSION

The copper base composite material is developed using a different type of reinforcement through powder compaction method. Figure 1a shows the microstructure of copper powder which is used as a matrix material and the average particle size of the copper particle is 30 ± 5 µm. It is a pure 99.9% Cu particle revealed in the spheroidal form with face centered cubic structure. The spheroidal shapes are highly recommended for powder compaction and enough susceptible to bear the compaction load. The copper base composite material with the hard reinforcement particles such as the silicon carbide, titanium carbide, zirconium oxide, aluminium – magnesium and graphene are as shown in Figure 1b. The morphological shape of the reinforcement is irregular in shape and the average size of the particle is as (30 ± 5 µm) matrix material. Irregular morphological shapes will help the reinforcement to fill the matrix material subsequently it will be supportive to reduce the porosity of the composite. Figure 2 shows the EDS spectra of the reinforcement particle indicating the purity of the particle. During compaction, the irregular particles will fit with the spheroidal particle and to completely gets compact. Subsequently the particle diffusion with the elevated sintering temperature will diffuse together to have a desired mechanical property.

Figure 1
(a) SEM image of pure Cu particle used for composite development. (b) Electron image of the reinforcement particle for comparison.

Figure 2
The backscattered electron image with the energy dispersive spectra (EDS) to confirm the reinforcement particle quality.

Table 2 shows the total weight of the composite powders along with the weight percentile of individual composition. Reinforcement weight percentage is fixed based on the research experience. The ceramic and metallic reinforcement along with the graphene helps to improve the base metal properties. The ceramic improves the hardness and the metallic with graphene will substantiate the desired metallurgical qualities without compensating the mechanical properties.

Table 2
Plan of Cu base composite with the detail on reinforcement particle.

TRIAL NO.	MATRIX MATERIAL	REINFORCEMENT wt.%	Wt. OF COMPOSITE POWDER
1	100 wt.% Cu	–	35g
2	90 wt.% Cu	7 wt.% SiC + 3 wt.% Gr	37.61 g
3	90 wt.% Cu	7 wt.% TiC + 3 wt.% Gr	39.25 g
4	90 wt.% Cu	7 wt.% ZrO2 + 3 wt.% Gr	40.17 g
5	90 wt.% Cu	7 wt.% AlMg + 3 wt.% Gr	38.93 g

The composite powder particles are mixed together using a ball milling process continuously for 60 minutes at a constant speed. The composite powders are ensured that the reinforcement particles and the base metal powders are perfectly mixed without agglomeration. Based on the industrial standard and to perform the test results (with respect to the ASTM standards) composite rods are developed through powder compaction [¹⁷]. Following the powder compaction, the samples are sintered in a box furnace. After sintering, the composite materials are furnace cooled and properties evaluation studies are performed.

The powder compaction samples after sintering process are sliced and polished to reveal the metallurgical microstructure and reinforcement nature. Figure 3 shows the microstructure of copper – graphene base composite with different reinforcements. The matrix material is the continuous phase with uniformly distributed reinforcement particles identified in the discrete phase throughout the microstructures. It is clear to infer that the matrix material has undergone the severe deformation to have a close bonding over the reinforcement (Figure 3i). Reference articles in the related combination of materials does also reports with similar morphological studies [¹⁸, ¹⁹]. Presence of carbides and / or carbon in the copper matrix is significantly different from the pure copper base sintered samples. Silicon carbide (SiC) and titanium carbide (TiC) reinforcements found to be an irregular phase identified throughout the matrix material (Figure 3ii and 3iii). The presence of TiC and graphene in copper matrix has better bonding compared to the SiC and graphene mixture. Influence of TiC has improved the bonding of the copper – graphene matrix compared to the SiC reinforcement [²⁰]. In the presence of ZrO² in the copper + graphene base metal found to be reactive and the reinforcement colour got interactive with the base metal (Figure 3iv). Subsequently the lightweight aluminium – magnesium (AlMg) particle found to be increased and the reinforcement has highly influenced the matrix material with large volume. Compared to the other three reinforcement particle the distribution of AlMg is dominating with the copper – graphene base composite material. in order to study the properties of the composite, the samples are prepared and evaluated for hardness, density and porosity for material characteristic evaluations.

Figure 3
Optical image of copper – graphene base composite with different reinforcements.

The sintered copper – graphene base composite samples are sliced and tested for mechanical properties such as hardness, density and porosity following the ASTM standards. The ASTM E92 is used to measure the micro hardness and following ASTM D792 for the density of the samples measured are given in the Table 3. From the experimental data the micro hardness of the pure copper matrix is measures as 51 Hv and the density of the samples is as 6.3 g/cc. It is also noticed that the porosity of the sample is 2.4% which is negotiable for a volume of pure composite material. The composite samples with different combination of reinforcements have wide range of differences in micro hardness and the density of the materials. The presence of graphene in the copper matrix will support to exfoliated the matrix material. Following process – sintering will help to improve the surface tension and metallurgical bonding of the material. Research on copper – graphene composite with silicon carbide and aluminium – magnesium reinforcements are as similar to the existing research [²¹, ²²]. The micro hardness is 37 Hv for both the reinforcement materials and the density for reinforcement of SiC is 7.25 g/cc and 3.95 for the AlMg material. Reduction in hardness in the Cu + SiC + Gr composite material is due to influence of graphene. Literature reported that the average (greater than 1% of graphene) will have a great impact over decrease over hardness; however, the presence of silicon carbide has substantially maintained the desirable hardness of the composite [²³]. The titanium carbide reinforced in the copper – graphene base composite has maximum hardness (50 Hv) and a density of 7.75 g/cc with an average of 2.6% porosity in the composite. Followed by the zirconium oxide having a micro hardness of 48 Hv and the density as 6.13 g/cc. The presence of zirconia reinforcement in the copper matrix has reduced the density as 93% compared to the pure copper / matrix material. It has been identified that the along with the density porosity of the Cu + ZrO₂ + Gr is maximum of 3.2% compared to the other combination of composite materials. Similar results reported by the existing researchers and confirmed that the presence of ZrO₂ in the copper has high hardness and average density [²⁴].

Table 3
Mechanical properties of copper – graphene base composite with different reinforcements.

TRIAL NO.	ELEMENT DETAILS	HARDNESS (HV)	DENSITY (g/cc)	POROSITY (%)
1	Cu	51	6.3	2.4
2	Cu + SiC + Gr	37	7.25	2.8
3	Cu + TiC + Gr	50	7.75	2.6
4	Cu + ZrO2 + Gr	48	6.13	3.2
5	Cu + AlMg + Gr	37	3.95	1.8

The machinability of copper base composites with different reinforcements are sliced using wire electro spark cutting process. Responses from the machining studies are evaluated in terms of surface roughness and surface topography. Figure 4 shows the average surface roughness value measured at different pulse duration. Copper is one of the best electrical conducting materials and used an eminent sourced for the energy transformation system. For the minimum pulse off time (10 µs) the energy transformation has induced the pure copper material to reveal a maximum surface roughness compared to the other composition. Reinforcements does not influence on energy conducting properties and do not involve in material removal. Since when there is a short pulse duration the energy transformation has not induced the material to get machined or vaporized. Instead, the resistivity of the material might be increased due to the influenced of reinforcement and leads to a poor transformation of the energy [²⁵, ²⁶]. Similarly for the maximum pulse duration the material might have prone to machining and the surface damage has induced the electro spark area to get vulnerable. For a maximum pulse duration of 30 µs the minimum roughness is measured with pure copper base metal and the SiC reinforced copper – graphene composite materials. The significance in particle reinforcement is less while compared to the wire electrical input process parameters over surface roughness. As the low surface roughness for the maximum pulse off time is recorded due to the maximum resistivity on energy conduction. The machined surface area during wire spark machining is prone to produce irrational surface topography due to partial metaling and vaporization of the material.

Figure 4
Average surface roughness value measured from the copper base composite material for different pulse duration.

During machining the pulse duration will influence the metal surface to metal and vaporize with respect to the intensity of the electro spark produced. For the longer pulse time influenced to produce less efficient machined surface. Surface area revealed with a micro pore and recast layers in the form of raggedness in the pure copper samples. The Figure 5i indicates the waviness of the machined surface and breathing of molten metal in the form of bubbles developed during the electro machining process. Literature confirms this as a mechanism of plasma energy getting collapsed during machining [²⁷]. In the Cu + TiC + Gr composites the machined surface revealed with a thermal cracks and micro pores (Figure 5iii). The titanium carbide is susceptible to the high energy plasma and the intensity of the plasma induced the composite to proliferate with a thermal crack. The zirconia and silicon carbide base composites are with high refractoriness and the recast layers reveal with a maximum spheroid over the machined surfaces. In contrast to all the above conditions, the presence of aluminium – magnesium reinforced composite has maximum craters. The soft AlMg which high in thermal radiation has undergone to diffusion and the composite revealed with pores and crates. That is the solubility of the material with respect to high heat energy produced during the electro spark machining process. The intensity of the electro spark produced during the machining has induced the material undergo the localised discussion and local thermal effect. The effect of thermal effect has been revealed in the surface topography of the machined surface.

Figure 5
SEM Image of copper – graphene composite with different reinforcement materials.

4. CONCLUSIONS

• The reinforcement found to be dispersed eventually in the matrix material with best metallurgical bonding. The presence of graphene and the wettability of the reinforcement has influenced the matrix material to have a best bonding. Presence of carbide reveals black in colour over the continuous phase of the light colour in the matrix material.

• Density of the TiC found to be maximum compared to pure copper and other carbide and oxide reinforcement. The titanium has influenced the copper metal to react and the copper grain stalled to grow denser than the pure metal. Hardness of the copper – graphene – titanium carbide has drastically increased the hardness of the composite.

• The presence of oxide in the copper base has induced the metal to reveal with more pores. Density of copper – graphene – titanium carbide composite is two-fold harder than the copper – graphene – aluminum magnesium composite material. Porosity of the AlMg reinforcement is less as the diffusivity is higher than the other reinforcements.

• Conductivity of the copper metal has similar surface topography with different pulse duration. However, the presence of reinforcement in the copper – graphene composite has undergone different morphological changes and roughness value increased for ZrO² reinforced composite followed by the TiC material. Due to the thermal radiation the soft AlMg has undergone surface damage and severity in pores and recast layers.

• From the machining studies it has been understood that the pure copper metal has uniform surface profile with minimum surface roughness. The surface reaction has induced due to the metallurgical reaction of the hard particle.

From the findings, the titanium carbide reinforced copper – graphene composite and zirconium – oxide reinforced copper – graphene composite has better performance than the other material. Subsequently this can be recommended for frictional components.

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Publication Dates

• Publication in this collection
  14 Feb 2025
• Date of issue
  2025

History

• Received
  26 Nov 2024
• Accepted
  09 Dec 2024