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Investigation of the compaction density of electromagnetic moulding of poly(ether-ketone-ketone) polymer powder

  • Fan Xu EMAIL logo , Hong Liu , Quantong Yao and Huixiong Wang EMAIL logo
Published/Copyright: December 19, 2024
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Abstract

During the moulding process of polymer composite powders, carbonisation often occurs owing to the insufficient ability to control temperature, thereby affecting the service performance of parts. This research studies the electromagnetic moulding (EM) of polymer powders at room temperature and demonstrated the deformation behaviour of poly(ether-ketone-ketone) (PEKK) powder particles for aviation under high-speed impact during EM. The orthogonal analysis method showed that the PEKK powder with a mass of 0.4 g had the highest compaction density of 1.242 when the discharge voltage was 8 kV. Discharge voltage was the most important parameter affecting compaction density, as discharge voltage increases, compaction density increases, but the mass is the opposite. The microstructure and hardness distribution in the specimens further demonstrate that discharge voltage is an important parameter affecting compaction density and provide process guidance for obtaining the high relative density of polymer products.

1 Introduction

With the rapid development of the aviation, aerospace, automobile, medical and health, military, and other fields, polymer composites, with the unique advantages of corrosion resistance, lightweight, amongst others, continue to improve and replace traditional industrial materials to achieve the goals of lightweight and intelligence. In the automotive field, numerous polymer composites are especially used to manufacture hybrid electric vehicles and electric vehicle batteries, reducing the weight of the vehicles to achieve lightweight design of automotive materials (1).

Polymer composites are a combination of polymer and at least one other material, integrating the physical and chemical properties of various materials. The matrix of polymer composites is divided into thermoplastic matrix and thermosetting matrix (2). Both matrix composites have been widely used in aerospace, aviation, biomedicine, automotive parts, electrodes, packaging materials, and other related fields owing to their good mechanical properties, insulation, corrosion resistance, and plasticity.

The previous researches (1,3) introduced the application of glass fibre-reinforced plastics to automobile braking systems, trunk lid and body reinforcement, automobile body parts, door panels, hoods, internal structures, engine frames, T-joints, signal transmission on aircraft, aircraft wings, safety facilities, and other parts, and showed the application prospect of polymer composites in the lightweight design of automobiles and aircraft. Lightweight is the primary characteristic of polymer composites, but their wear resistance and heat insulation properties make them widely used considerably. Phenolic resin and carbon-reinforced fibre composites can be used as fireproof and heat insulation materials, such as for the heat shield of spacecraft (4). Carbon-reinforced epoxy resin composites with metalloid mechanical properties are extensively utilised in the automotive field because of their advantages of lightweight, extreme strength, high rigidity, and recyclability (5). Each polymer compound is applied to various fields with its unique physical and chemical characteristics. Poly(aryl-ether-ketone) (PAEK) is a family of polymer composites broadly adopted for military and civilian uses. Particularly, poly(ether-ketone-ketone) (PEKK) has superior properties when combined with carbon-reinforced fibre because of its high mechanical properties and temperature stability (6). Additionally, PEKK can be used as the material of high-temperature components in aviation (7). Polyetherimide-based composites are also commonly used in aviation owing to their excellent fire resistance (8).

Artificial organs made of aerospace poly(ether-ether-ketone) composite materials as implant materials have been widely used in the operation of key parts of the human body (9,10). PEKK, which is another important polymer material in the PAEK family, has become a new dental implant and dental restoration material (11). In consideration of the heat conduction, wear resistance, and corrosion resistance of polymer composites, the corresponding materials are added in accordance with the demand to make the polymer composites have the properties of electric conduction, heat conduction, magnetic conductivity, and energy storage. They have also been widely used in electrode devices (12,13), electromagnetic interference shielding devices (14,15,16,17), sensors (15,18,19), packaging materials (19), and energy storage devices (20).

The quality of polymer and its composite products is not only limited by the material preparation technology but also affected by the moulding manufacturing technology. Increasing studies have addressed the moulding and application of PEKK and its composite materials, and they have gradually become a research hotspot in recent decades (15). The main moulding methods for PEKK composites include additive manufacturing, hot press moulding (21,22,23), spark plasma sintering (SPS) (24), injection moulding (25,26), and extrusion moulding (27). In a previous study, the research group used hot pressing to form graphene/PEKK composites with different graphene contents. Hot pressing had a long pressure holding time and low production efficiency. In the aforementioned moulding methods, moulding temperature is an important factor affecting the compaction quality of the specimens. Therefore, a temperature-independent moulding method is needed to meet the compaction density of powder metallurgy products.

This study discusses the effect of different discharge voltages on the moulding quality of PEKK polymer powders by using electromagnetic equipment (EME) is discussed. Section 2 introduces the performance of PEKK polymer powder, EME, and powder processing. Section 3 mainly presents the experimental results and discussion, test parameter optimisation, and quality evaluation. The orthogonal analysis method is used to identify reasonable process parameters to obtain the maximum factors affecting compaction density. Macro and micro tests are also conducted to prove the effect of discharge voltage on moulding quality. In the future, PEKK specimens obtained by electromagnetic moulding (EM) will be used in medical health and organ transplantation because of compaction density.

2 Experimental method

2.1 Material performance

PEKK is a high-performance thermoplastic from the PAEK family. It has high thermal stability, chemical resistance, and mechanical properties (28). The PEKK powder was observed using an Olympus optical digital microscope (DSX500, Shanghai Liyang Industrial Co., Ltd, Shanghai, China). Additionally, a differential scanning calorimeter (STA449–C, NETZSCH, Free State of Bavaria, Germany) test was conducted. Its high glass transition temperature (T g = 140°C) and melting point (T m = 320°C) make it suitable for aeronautical applications (29), which is extremely close to the products of the OXPEKK series. Given the limited conditions of the research group, we adopted other physical properties of the OXPEKK products, made minor corrections and found that the density of the PEKK was 1.35 g·cm−3, yield strength was 138 MPa, and elastic modulus was 4,500 MPa (29).

Figure 1(a) presents the morphology of the PEKK specimens obtained using the SPS method by scanning electron microscope (SEM). Figure 1(b) shows the morphology of the PEKK specimens obtained via an EM process through SEM analysis. The comparison of two types of microstructure indicates that powder compaction with good uniformity of the quenched section is achieved mainly through EM. However, some large holes can be observed in the cross-section of the SPS method, suggesting that the EM method is a good method to improve compaction density.

Figure 1 
                  Microstructure of the PEKK under different stages: (a) PEKK by SPS technology and (b) PEKK by EM technology.
Figure 1

Microstructure of the PEKK under different stages: (a) PEKK by SPS technology and (b) PEKK by EM technology.

2.2 EME

The electromagnetic pulse powder compaction technology is a rapid prototyping method, which impinges powders in the form of stress waves at high speed. During moulding process, the powder particles undergo elastic–plastic deformation and bond to improve the mechanical properties. Moulding speed is controlled by regulating the discharge voltage and capacitance to avoid the noise pollution caused by the heavy hammer impact and improve moulding quality.

Previous studies have mainly focused on powder materials with good electrical and thermal conductivity, such as metals, metal composites (30,31,32,33), and inorganic nonmetallic materials (34,35,36,37). However, only a few researchers have studied the EM of polymers and their composites. Wang et al. (38) used the electromagnetic pulse powder compaction technology to study the moulding of a graphene/PEKK composite powder and obtained the influence law of process parameters on the moulding quality of graphene composite. Our research group conducted EM research on the matrix material PEKK to seek appropriate process parameters and reduce research costs.

The ARCHIMEDES VEMP–80 EM equipment developed by Archimedes Industrial Technology Co., Ltd. is shown in Figure 2(a). The moulding device and tool are presented in Figure 2(b) and (c), respectively. The driving plate is placed above the pressure block to contact the flat coil. The flat coil is connected to the capacitor through the wire, and the moulding device is pressed and kept fixed by the hydraulic device. The working coil is a flat spiral coil wound by a red copper wire, with a cross-sectional area of 2 mm × 20 mm. A key component of the EM equipment is the driving plate. During discharge process, the driving plate generates an induced magnetic field, which is opposite to the magnetic field generated by the coil. The driving force of the driving plate is formed, which promotes the movement of the pressing block and compacts the PEKK powder. The material of the driving plate is 45# steel. If the punch with a 10 mm diameter is in direct contact with the drive sheet and misaligned, it is easy to be broken, leading to the failure of the die. Therefore, the pressing block is set up, and the concave die assembly is extended. The die is made of hardened alloy steel to improve the hardness of the die.

Figure 2 
                  EME: (a) The EM equipment; (b) the moulding device and tool; and (c) the geometric size of the tool.
Figure 2

EME: (a) The EM equipment; (b) the moulding device and tool; and (c) the geometric size of the tool.

2.3 PEKK powder processing

The PEKK powder is placed in the mould, and then the charging voltage is set thereafter. A control cabinet is used for charging. When the current flows through the flat coil, the induced magnetic field will be formed near the coil. Electromagnetic induction forms the induced magnetic field near the driving plate, and the two induced magnetic fields interact to generate a strong pulse force transmitted to the driving plate. Thereafter, the driving plate pushes the punch to realise a high-speed compaction of the PEKK powder by inertial force. The driving plate under the plate coil generates eddy currents under the action of the induced magnetic field, forming a closed loop, and then it will start working.

Electromagnetic compaction is a high-speed impact moulding technology with fast loading speed. The current detection system uses a Roche coil without integrator to measure. Input current is proportional to output voltage signal, output sensitivity is 6.8 mV·kA−1, and the working frequency is 50 Hz. The relationship between input current and output voltage is as follows:

(1) i ( t ) = 1,000 u ( t ) 6.8 × 50 × 1,000 = 2,941 u ( t )

The system shown in Figure 3(a) is used to test discharge currents at discharge voltages of 7, 8, and 9 kV, and the test results are demonstrated. The peak value of the first pulse appears near 0 because the phase of the measured sine wave is mainly ahead of the actual value owing to the influence of the working frequency of the Roche coil without integrator. Additionally, the phase lead is 90° when the working frequency is 50 Hz. With an increase in discharge voltage, the peak of discharge current gradually increases, while the discharge period is unchanged. When discharge time is about 2 ms, the energy release tends to be stable. At this time, the deformation of powder particles under the action of inertial force changes from elastic deformation to plastic deformation, and they eventually achieve bonding.

Figure 3 
                  Discharge current and magnetic field force under different discharge voltages: (a) discharge current and (b) electromagnetic force.
Figure 3

Discharge current and magnetic field force under different discharge voltages: (a) discharge current and (b) electromagnetic force.

Electromagnetic force is measured using the pressure sensor, and a strain gauge is encapsulated in the sensor with polyvinylidene fluoride glue. Charge signal is collected using a data acquisition instrument and transmitted to a computer for storage and display. The sensor used in the test has a measuring range of 900 kN and sensitivity of 0.036 pC·N−1. Charge amplifier is the VK102 product of Shenzhen Weijingyi Electronics Co., Ltd. Charge input range is 0 to ±5,000 pC, and the sensitivity is 100 pC/100 mV. Therefore, the relationship between impact force and voltage signal is as follows:

(2) F = U / 0.036

where F represents the impact force in N and U indicates the output voltage in mV.

Figure 3(b) shows the electromagnetic force distribution under discharge voltages of 7, 8, and 9 kV, and its period is consistent with the period of the measured discharge current. Impact force is the largest at the first peak and rapidly decays thereafter. After the second peak, the decay rate gradually slows down. Thus, the first peak plays a major role in powder compaction. With an increase in discharge voltage, the electromagnetic force generated by inertial force increases linearly. Pressure sensors can only measure pressure but not tension, so the negative half axis of the electromagnetic force is zero. When the discharge time reaches about 2 ms, the electromagnetic force changes the deformation of the PEKK particles from elastic deformation to plastic deformation, similar to the discharge current, and bonding between powder particles is achieved. The utilisation rate of the EME is very low, not even over 15%. Hence, the measured electromagnetic force during the test is often considerably higher than the calculated value. Figure 4 shows specimens of different sizes for the EM of the PEKK polymer materials, which are completed under different discharge voltages and mould sizes.

Figure 4 
                  The rods under different discharge voltages and the sheets under different discharge voltages and same weight.
Figure 4

The rods under different discharge voltages and the sheets under different discharge voltages and same weight.

3 Results and discussion

3.1 Compaction density

In the process of EM, the relative compaction densities of specimens under different discharge voltages and geometry sizes in the mould conditions are compared, as shown in Figure 5. As discharge voltage increases, compaction density increases. However, the comparison of 30 mm specimens with 10 mm specimens indicates that the compaction density of the former is lower than that of the latter. Electromagnetic force is the impact force applied to the strain gauge, and pressure directly acts on the specimen particles with a diameter of 30 mm. That is, the strain per unit area is less than that of the specimen with a radius of 10 mm. Theoretically, particle deformation does not reach the plastic deformation stage, or there is still a part of elastic deformation. Thus, compaction density is markedly high under the same discharge voltage.

Figure 5 
                  Electromagnetic force and relative density distribution on the rod under different discharge voltages.
Figure 5

Electromagnetic force and relative density distribution on the rod under different discharge voltages.

The inertial force of high-speed impact causes particles to undergo completely inelastic deformation, bonding force between particles is greater, and the essence of the plastic deformation of particles is the inertial force per unit volume. The low utilisation rate of equipment in the EM is still the difficulty in improving equipment performance. Compaction density is the main influencing factor of the mechanical properties and other properties of products. The relationship between the density and morphology of products is evaluated using SEM.

3.2 Optimisation of processing parameters

A computer control platform built in the laboratory is used to process various polymer materials. Energy loss in the test process is large, but the moulding quality is good. To improve efficiency, moulding process parameters are optimised before the development of large quantities of products, and the most important factors affecting the density of products are determined. This study adopts the orthogonal analysis method to optimise the process parameters for EM PEKK polymer materials. Additionally, the current research provides theoretical and experimental bases for the engineering application of the PEKK products.

An effective design method is needed to reduce the experimental cost and time (23). Several factors and levels should be considered when optimising the parameters during the EM powder process. Orthogonal design is a method that is mainly used to study multiple factors and levels. This design method is uniformly dispersed, neat, and comparable, thereby making each design highly representative. The selection of representative points from the comprehensive design can fully reflect the impact of different levels of each factor on the design result with minimal time cost. To facilitate the research, a suitable orthogonal table should be constructed (20). Discharge voltage, the weight of the PEKK powder, and holding time are important factors influencing compaction density during EM process. These factors are independent parameters. This study disregards temperature and discharge time. Therefore, these parameters should be predicted before the orthogonal analysis to determine an approximate range. This research establishes three three-level factors in the orthogonal array used to optimise the parameters during EM process (Table 1 (L9(34)). A group of nine parameter combinations should be simulated to find the optimal moulding parameters according to the orthogonal array (Table 2).

Table 1

Parameters and the levels

Weight (g) Hold time (s) Discharge voltage (kV)
1 0.4 10 6
2 0.5 15 7
3 0.6 20 8
Table 2

Results of orthogonal design

No. A B C D
1 1 1 1 0.998
2 1 2 2 1.132
3 1 3 3 1.242
4 2 1 3 1.222
5 2 2 1 0.962
6 2 3 2 1.160
7 3 1 2 1.104
8 3 2 3 1.233
9 3 3 1 0.927

The most important factors affecting electrical conductivity during EM process are shown in Table 3. K a denotes the sum of the test indicators (a denotes level (1, 2, 3)), i denotes level (1, 2, 3), j denotes factor (A, B, C), k ij is equal to K ij divided by 3, and rank is equal to the maximum (k ij ) minus the minimum (k ij ). Table 3 presents the extreme difference analysis of compaction density during EM process. The orthogonal analysis is used to establish the influence trend of discharge voltage on compaction density (Figure 6 and Table 3). In EM process, suitable moulding parameters (A 1 B 3 C 3: 0.4 g, 20 s, 8 kV) are used to obtain the bars of the PEKK composite with 1.242 compaction density.

Table 3

Extreme difference analysis of the compact density

No. A B C D
1 1 1 1 0.998
2 1 2 2 1.132
3 1 3 3 1.242
4 2 1 3 1.222
5 2 2 1 0.962
6 2 3 2 1.160
7 3 1 2 1.104
8 3 2 3 1.233
9 3 3 1 0.927
K 1 3.372 3.324 2.887
K 2 3.344 3.327 3.396
K 3 3.264 3.329 3.697
k 1 1.124 1.108 0.962
K 2 1.115 1.109 1.132
K 3 1.088 1.110 1.232
Rank 0.036 0.002 0.270
R 2 3 1
Figure 6 
                  Effect of process parameters on compact density.
Figure 6

Effect of process parameters on compact density.

3.3 Microstructure analysis

Figure 7 shows the morphology of the PEKK specimens formed by electromagnetic force at different discharge voltages. When the discharge voltages are 5 and 6 kV, the distance between particles is not uniform, and there is a clear boundary. When the discharge voltage increases (i.e., the energy increases to 7 and 8 kV), the boundary between particles is clearly blurred, the distance between particles is infinitely close and the particles experience the elastic–plastic deformation-bonding evolution. The particles collide with one another in a completely inelastic way and stick together. As mentioned in the previous orthogonal analysis, with an increase in discharge voltage, compaction density increases, the particles are shaped by high-speed impact and the deformation direction is perpendicular to the electromagnetic force. In the EM process, infrared monitoring shows no temperature change in the moulding process. The melting phenomenon does not occur, and deformation belongs to cold impact moulding. Thus, there is no carbonisation phenomenon during the EM to ensure the initial performance of the material preparation.

Figure 7 
                  SEM analysis of the rod under different discharge voltages.
Figure 7

SEM analysis of the rod under different discharge voltages.

The completely inelastic collision of the PEKK particles during the EM makes the particles form solid joints. Its essence is that under the action of the inertial force of EM, when discharge energy is about to disappear, the inertial force generated by the stress wave between the particles causes permanent plastic deformation, and a firm adhesive force is generated between them. When discharge voltage is 5 kV, the quenched surface is not uniform; when the discharge voltage is 8 kV, the quenched surface is uniform. This result proves that particle deformation is uniform, and the density is high at high voltage. The microstructure of the PEKK specimens shows the deformation law of particles in the high-speed impact and explains the root cause of the increase in compaction density. The SEM analysis demonstrates that without PEKK carbonisation, PEKK polymer powder is formed by high-speed impact. After curing treatment, adhesive force between its particles will be further increased, reducing the fracture stress caused by the high-speed impact at the bond and ensuring the mechanical performance of the PEKK specimen.

3.4 Compressive hardness

Compressive hardness is an important index for evaluating the compaction density of the PEKK specimen. Specimen quality is determined by examining the compaction density, which is specifically manifested in engineering as compressive hardness. Figure 8 shows the compressive hardness of the specimens with a diameter of 10 mm under different discharge voltages. PEKK represents the compressive hardness of the specimens under different discharge voltages, and the local flanges of the good specimens are corrected before hardness testing. As the discharge voltage increases, compaction density increases and compressive hardness also increases.

Figure 8 
                  The compressive hardness under different discharge voltages (5, 6, 7, and 8 kV).
Figure 8

The compressive hardness under different discharge voltages (5, 6, 7, and 8 kV).

According to the microstructure analysis under different discharge voltages, as shown in Figure 7, compaction density is low, and binding between particles is incomplete at 5 and 6 kV under cold stamping. With increases in discharge voltage and energy, collision velocity between particles is increased to achieve completely inelastic collision and bonding, Additionally, the compressive hardness is further improved. Note that when discharge voltage is 4 kV, the hardness of the PEKK specimen cannot be tested at room temperature. Moreover, taking out of the mould completely is generally difficult, as shown in the red dotted line. In the future, curing temperature is selected for curing treatment to improve the hardness of specimens.

With an increase in discharge voltage, compaction density and compressive hardness are increased, and bonding force between particles is enhanced.

4 Conclusion

A computer control platform built in the laboratory was used to process PEKK powder specimens under different technological parameters. The variation law of the main parameters affecting the density of the PEKK powder moulding was obtained, providing a reliable theoretical and experimental bases for future research on the industrialisation of other polymer products. The following conclusions were obtained through experimental research.

  1. PEKK specimens with high compaction density were obtained via the EM method. The reasonable process parameters and factors affecting the density of high–speed impact powder moulding were determined through orthogonal analysis. The optimal compaction density of 1.242 was obtained by selecting the A1B3C3 combination.

  2. The compressive hardness of the PEKK powder moulded specimens under different discharge voltages increased from 0.35 GPa to 1.2 GMPa. In future research, the combination moulding method can be used to obtain specimens with high compaction density by EM. Moreover, the adhesive force between particles can be improved after curing treatment to expand the engineering application prospect of products.

  3. From the orthogonal analysis, discharge voltage was the most important parameter affecting compaction density. With an increase in discharge voltage, the compaction density of the PEKK polymer specimens increased. The comparison of the microscopic morphology of specimens at 5, 6, 7, and 8 kV indicated that when discharge voltage was 5 kV, the distance between particles on the quenching surface was uneven, and plastic deformation was incomplete. However, when discharge voltage reached 8 kV, particles on the quenching surface were clearly bonded.

Acknowledgements

This work was supported by the: University of Science and Technology Liaoning Talent Project Grants (601010386).

  1. Author contributions: Funding acquisition: Fan Xu; writing – original draft: Fan Xu; validation and investigation: Fan Xu; data curation, formal analysis, and preparation of materials: Hong Liu and Huixiong Wang; preparation of materials: Quantong Yao and Huixiong Wang.

  2. Conflict of 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 study.

  3. Data availability statement: Data sharing is not applicable to this article as no datasets were generated or analysed during the current study.

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Received: 2024-04-28
Revised: 2024-05-31
Accepted: 2024-06-01
Published Online: 2024-12-19

© 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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