Startseite Facile rheological route method for LiFePO4/C cathode material production
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Facile rheological route method for LiFePO4/C cathode material production

  • Meidiana Arinawati , Anjas P. Hutama , Cornelius S. Yudha , Mintarsih Rahmawati und Agus Purwanto EMAIL logo
Veröffentlicht/Copyright: 5. Mai 2021
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Aus der Zeitschrift Open Engineering Band 11 Heft 1

Abstract

LiFePO4/C cathode material is largely used in Li-ion batteries due to its low toxicity, nonhazardous and high stability features. A facile and simple approach is proposed in LiFePO4/C production using low-cost materials. The effect of carbon addition during the formation of LiFePO4/C was investigated. Based on the XRD and FTIR analyses, olivine-structured LiFePO4/C cathode material was successfully obtained via methanol-based rheological method. The SEM result showed that the material has micron-sized polyhedral shape. The electrochemical performance tests were conducted in an 18,650-type cylindrical battery. The charge–discharge performances were tested at a voltage range of 2.2–3.65 V using charge and discharge rate of 1C. Based on the charge–discharge test, LiFePO4 with 30% carbon addition has the highest specific capacity of 121 mA h/g with excellent cycle and rate performance as a result of successful carbon compositing in LiFePO4 material. This approach is promising to be adapted for mass production of LiFePO4/C.

Keywords: LiFePO4 ; rheology; composite; synthesis; Li-ion batteries; cathode

1 Introduction

Batteries are an electrochemical device with an ability to alter the chemical energy into electricity and thus often found in wireless electronics as energy storage. Based on its rechargeability, batteries can be classified into two types, namely, primary battery and secondary battery. A secondary battery is rechargeable, meaning it can be repeatedly used with external energy source. At this moment, the most promising secondary battery is lithium-ion battery (LIB) [1,2,3,4].

Inside an LIB, four main components are anode, cathode, separator and electrolyte. The capacity of LIBs is largely dependent on the cathode materials as the host network of an Li-ion as the charge carrier. Therefore, high-capacity cathode materials with high volumetric and gravimetric density are highly needed in an LIB cell. Many types of cathodes are used in LIBs, including lithium cobaltate (LiCoO2) [5], lithium manganese oxide (LiMn2O4) [6,7], lithium nickel cobalt aluminum oxide (LiNi0.8Co0.15Al0.05O2) [8,9,10] and lithium iron phosphate (LiFePO4) [11]. Spinel-type LiMn2O4 offers economical features; however, it has low gravimetric and volumetric capacity. Layered structure of LiCoO2, LiNi1/3Co1/3Mn1/3O2 and LiNi0.8Co0.15Al0.05O2 has higher capacity and density of all types; however, the safety issues and high-cost raw material are the main concerns in adapting such cathode material. Among other types, LiFePO4 material is a balanced choice, with features such as high thermal stability, environmentally friendly, long lifespan and inexpensive starting materials, for example, iron and phosphate have high availability with nontoxic properties. On the other hand, it has sufficiently high theoretical capacity (170 mA h/g) [12].

Various synthesis routes to obtain LiFePO4 have been reported in previous studies, such as (i) solid state reaction, (ii) carbothermal reduction method, (iii) Pechini’s/sol–gel method, (iv) microwave synthesis method, (v) coprecipitation method, (vi) hydrothermal/solvothermal synthesis method, (vii) freeze–drying process, (viii) nonthermal synthesis and so on [13,14,15]. Even though numerous studies on LiFePO4/C synthesis have been performed in the past two decades, large-scale production of LiFePO4/C is rarely discussed in previous reports. The lack of mass production-oriented studies creates a gap between research and industrial application. The removal of this gap or a research that creates a bridge between lab-scale and industrial-scale application is a crucial step toward a more economically feasible LFP/C product. Therein, in this study, we synthesized LiFePO4/C via a rheological phase reaction method from pretreated highly available iron sulfate. Rheological phase method utilized solvents such as water and organic solvent to assure raw material distribution during the mixing process; thus, a final homogenous precursor can be easily obtained. The effect of carbon content on the physiochemical characteristics of LiFePO4 was deeply investigated. The raw materials are in technical grade and the production of LiFePO4 is in pilot plant scale (150 g per batch). Since low-grade iron sulfate precursor was used, we provide a simple, economical and facile pretreatment process to obtained better characterized and high-purity precursor. The as-produced LiFePO4/C powders were used as the cathode material in an 18,650-type cylindrical LiFePO4/artificial graphite battery. Such efforts have never been reported in previous studies.

2 Methodology

2.1 LiFePO4 synthesis

Technical-grade FeSO4·7H2O of 280 g was dissolved in 1 L of distilled water and then technical-grade HCl 32% of 30 mL was added slowly to the technical FeSO4 solution until the solution turned green under vigorous stirring for an hour and allowed to age for another hour. Iron sulfate and hydrochloric acid were obtained from Hunan, China, and Asahi, Indonesia, respectively. The green solution is filtered using a vacuum filter.

One liter of 1 M FeSO4 solution was heated at 60℃ and stirred under 700 rpm speed. Eight hundred millilitre 1 M oxalic acid (Yuanping Changyuan Chemicals, China) and 25% ammonia (Merck, Germany) were slowly transferred into the FeSO4 solution while maintaining the temperature and pH of 60℃ and 2, respectively, under vigorous stirring for 2 h. Yellow precipitate was allowed to settle while brownish solution was carefully removed. The FeC2O4 precipitate was washed several times until the pH reached 6–7, filtered using vacuum filter and store in an oven for a night.

To make the cathode material, 157 g of LFP, 42 g of LiOH (Leverton, India), 100 g of H3PO4 (Brataco, Indonesia) and 100 mL of methanol (Brataco) were mixed using an overhead stirrer at 700 rpm for 2 h. Next 180 g of FeC2O4 was put into the slurry and further stirred for another 2 h. Homogeneous slurry was dried overnight in an oven at 120°C to obtain dried LFP precursor. Various percentages (0, 1, 3, 5, 7, 10 and 30% w/w) of commercial glucose were mixed with the dried precursor using mortar and pestle. The final LFP precursor composite was heated in a tube furnace at 700℃ for 12 h under a flow of nitrogen gas. The LFP product produced was ground using mortar and pestle and sieved using 100 mesh filter. The overall steps are displayed in Figure 1.

Figure 1 Flow diagrams of LiFePO4 electrode production.
Figure 1

Flow diagrams of LiFePO4 electrode production.

2.2 Material characterization and electrochemical performance

The crystal structure of FeC2O4 and LiFePO4/C samples was examined using mini-diffractometer (MTI, USA) at 2θ range of 17–67°. The morphology of the particle was investigated using scanning electron microscopy (SEM; JEOL JSM-6510LA, Japan). The surface chemistry of the particles was studied using FTIR spectroscopy (Shimadzu FTIR, Japan). The electrochemical performance tests were conducted in 18,650 cylindrical batteries using graphite as the counter anode. The LFP electrode sheet was prepared by coating a mixture of LFP:AB:KS6:PVDF of 80:5:5:10 in N-Methyl-2-Pyrrolidone solvent on both sides of Al foil with a cathode coating thickness of 200 µm. The coated sheet was dried and assembled in cylindrical cells using cylindrical cell assembly equipment (MTI). LiPF6 dissolved in 3:7 EC:DMC was used as the electrolyte. The cells were aged for a day and charge–discharged using 0.1C rate at voltage window of 2.2–3.65 V using Neware Battery Analyzer (Neware, China). Electrochemical impedance spectroscopy (EIS) analysis was performed using NuVant EZ-ware (Nuvant System Inc., USA).

3 Results and discussion

3.1 Iron sulfate purification

In this study, the production of LiFePO4/C precursors was carried out using the coprecipitation method with materials in the form of technical FeSO4. But before the technical-grade FeSO4 was used, it should be reduced with HCl acid. This is because the technical-grade FeSO4 obtained from local vendor oxidizes to form Fe3+(Fe2(SO4)3 and Fe2O3) (Figure 2(a)), and the raw material is not completely soluble, becoming reddish yellow, thereby causing uncertainty in the Fe content [16]. The occurrence of reduction reaction is confirmed when a green solution is formed, which is predicted to be similar to the reductive leaching process of metal oxide as seen in equation (1). In the acidic environment, the formation of Fe3+ is inhibited; therefore, a stable Fe2+ solution is obtained.

(1) Fe ( aq ) 3 + + Cl ( aq ) − ( reddish yellow ) → Fe ( aq ) 2 + + 1 / 2 Cl 2 ( g ) ( green )

Figure 2 (a) FeSO4 precursor and (b) pretreated yellow FeC2O4 precursors.
Figure 2

(a) FeSO4 precursor and (b) pretreated yellow FeC2O4 precursors.

3.2 Synthesis of Fe2C2O4·2H2O powder

FeSO4 solution of 1 M was reacted with 1 M oxalic acid solution and ammonia solution with continuous stirring and heating for 1 h at 60℃. In this case, FeSO4 functions as a source of iron, ammonia as a regulator of pH and oxalic acid as a precipitant. During the stirring process, yellow precipitate was formed (Figure (2b)). The precipitate was filtered and tested for its characteristics by XRD and FTIR tests.

Figure 3 shows the results of the XRD spectra of FeC2O4 powder. The peaks in the diffraction pattern correspond to the diffraction peaks of FeC2O4 (JCPDS 72-1305) [17]. It can be concluded that the solids formed are indeed iron oxalate powders. The peaks in the diffraction pattern have a high intensity. This indicates that the solid has highly crystalline properties [18].

Figure 3 XRD pattern of FeC2O4 precursors.
Figure 3

XRD pattern of FeC2O4 precursors.

Surface properties of the FeC2O4 sample were analyzed using FTIR and SEM. FTIR determined the groups formed in FeC2O4 particles (Figure 4(a)). Based on the result, H2O antisymmetric stretching modes 3,410–3,395/cm; C‒C group appears in the range of antisymmetric stretching modes 2,123/cm; C‒O appears in the range of antisymmetric stretching modes 1,646–1,655/cm; and C‒O‒H appears in the range of antisymmetric stretching modes 1,334–1,320, 1,431–1,438 and 665–667/cm, while the C–O group appears in the range of antisymmetric stretching modes 1,382–1,036/cm [19]. The high H2O peak indicates that the precipitate formed is in hydrate form. The overall reaction of FeC2O4·2H2O precursor formation is presented in equation (2). Figure 4b shows the micron size of FeC2O4 particle and is of rod shape.

(2) FeSO 4 ( aq ) + 2 NH 4 OH ( aq ) + H 2 C 2 O 4 ( aq ) → FeC 2 O 4 ⋅ 2 H 2 O ( s ) + ( NH 4 ) 2 SO 4 ( aq )

Figure 4 (a) Infrared absorption spectra (FTIR) of FeC2O4·2H2O precursor; (b) SEM images of FeC2O4 particle.
Figure 4

(a) Infrared absorption spectra (FTIR) of FeC2O4·2H2O precursor; (b) SEM images of FeC2O4 particle.

3.3 Production of LiFePO4/C cathode materials

The reactions that occur in the formation of LiFePO4 and LiFePO4/C are presented, respectively, in equations (3) and (4).

(3) LiOH ⋅ H 2 O ( s ) + FeC 2 O 4 ⋅ 2 H 2 O ( s ) + H 3 PO 4 ( aq ) → LiFePO 4 ( s ) + 2 CO ( g ) + 3 H 2 O ( g ) + 3 / 2 H 2 ( g )

(4) LiOH ⋅ H 2 O ( s ) + FeC 2 O 4 ⋅ 2 H 2 O ( s ) + H 3 PO 4 ( aq ) + a C 6 H 12 O 6 ( s ) → LiFePO 4 ( s ) + b C ( s ) + c CO 2 ( g ) + d H 2 O ( g )

3.3.1 Structural analysis of LiFePO4/C samples

The results of the XRD analysis of LiFePO4 by rheological method are shown in Figure 5. The peaks in LiFePO4/C products are in accordance with the peaks in commercial LiFePO4/C (PDF (81-1173)) [14]. The peaks in LiFePO4 0% C XRD patterns are clearer than the other samples. This is because, the higher the carbon content in LiFePO4/C products, the lower the intensity, so that the peak produced will be lower [20].

Figure 5 Results of XRD LiFePO4/C.
Figure 5

Results of XRD LiFePO4/C.

3.3.2 FTIR analysis

Figure 6 shows the FTIR spectra of LiFePO4/C material. Two function groups can be observed, namely, the OH− bond and PO4 3− group. But the OH− bonds that are formed are not so clear that it can be ascertained that the particles formed are really LiFePO4/C. The H2O bond appears in the range of antisymmetric stretching modes 3,000–3,500/cm, while the PO4 3− group appears in the range of antisymmetric stretching modes from 1,000–1,200 to 400–560/cm [21].

Figure 6 FTIR spectra of LiFePO4/C at various carbon additions.
Figure 6

FTIR spectra of LiFePO4/C at various carbon additions.

3.3.3 SEM analysis

SEM analysis was used to examine the surface morphological properties and the size or diameter of LiFePO4/C particles. Particle measurement was randomly conducted. The SEM image of LiFePO4/C at various carbon additions is displayed in Figure 7 at 5,000× magnification. Based on the SEM analysis result, with increasing carbon content addition, the submicron-sized primary particles become smaller. Smaller particle size is favorable, since it has a large surface area increase in the Li-ion diffusivity during intercalation and de-intercalation processes. Several particles appear to be of polyhedral shape with grains that can be clearly observed [22].

Figure 7 SEM images of LiFePO4/C sample with carbon additions of (a) 0%, (b) 7%, (c) 10% and (d) 30%.
Figure 7

SEM images of LiFePO4/C sample with carbon additions of (a) 0%, (b) 7%, (c) 10% and (d) 30%.

3.3.4 Specific capacity test of LiFePO4/C samples in a cylindrical cell

Electrochemical performance tests were carried out on cylindrical cells with LiFePO4/C sample as the cathode and graphite as the counter anode. A formation process using 0.05C current rate was applied in every cells before further cycled at higher current rate. The specific capacity of LiFePO4/C at 1C current rate in 18,650 cylindrical batteries can be seen in Figure 8. The resulting capacity of each sample is still low when compared with the theoretical capacity of LiFePO4/C batteries (165 mA h/g). This is due to the fact that tests were conducted using the full-cell method (non-Li-based anode), while the theoretical capacity is obtained by the half-cell method (Li metal as an anode) [23]. The capacity of the samples increases with the increase in the addition of carbon sources of up to 30%. It is predicted that with high carbon content, better LiFePO4 material is achieved. Based on Figure 8, the highest specific capacity of 121 mA h/g is exhibited by LFP 30% C. The specific capacity of commercial LiFePO4 is lower than that of LFP 30% C and LFP 10% C. This phenomenon proves that such method is promising and is ready to be adapted at industrial scale [24]. More carbon addition and surface study are necessary to be investigated in the future projects.

Figure 8 Specific charge–discharge capacity of LiFePO4/C samples.
Figure 8

Specific charge–discharge capacity of LiFePO4/C samples.

Figure 9a presents the cycle performance of LFP/C samples and commercial LFP at 1C. The capacity retention of LFP 7% C, LFP 10% C and LFP 30% C after 50 cycles is 58.4, 85.2 and 89.5%, respectively. This proves that addition of carbon during the synthesis process significantly improves the cycle performance. Figure 9b presents a comparison of LFP/C with 7, 10 and 30% carbon rate performance with a commercial LiFePO4 obtained from MTI. Based on the picture, the higher the charge and discharge currents, the lower the specific discharge capacity in both samples. At higher charge–discharge rate, the ability of Li ions to move decreases due to the conductivity and diffusivity of the material. The reduction in the capacity of the LiFePO4/30% C sample is still higher than that of commercial LiFePO4, this is due to the high carbon content increasing the conductivity of the material [24].

Figure 9 (a) Cycle performance and (b) rate performance test of LiFePO4/C at various carbon additions.
Figure 9

(a) Cycle performance and (b) rate performance test of LiFePO4/C at various carbon additions.

3.3.5 EIS analysis

Figure 10 presents the EIS test result in the form of Nyquist plot. Based on the figure, it can be observed that each sample does form a semicircle curve. However, the sample with the lowest semicircle diameter is LFP 30% C, while LFP 7% C has the largest semicircle diameter. This shows that the LFP 30% C sample has good Li diffusivity and conductivity due to its carbon content [25]. This phenomenon is also the reason that LFP 30% C sample has good cycle and rate performance (Figure 9).

Figure 10 Nyquist plot of LiFePO4/C samples in cylindrical cells.
Figure 10

Nyquist plot of LiFePO4/C samples in cylindrical cells.

4 Conclusion

A large-scale (pilot-scale) production of LiFePO4/C is successfully conducted via methanol-based rheological method. In this study, the addition of carbon source during the formation of LiFePO4 had an effect on the conductivity of the material. Low-grade cheap FeSO4 can be easily purified by adding HCl into the solution. The formation of FeC2O4·2H2O is ensured using simple batch oxalate precipitation confirmed by XRD and FTIR analyses. The XRD patterns of all LiFePO4/C samples are well indexed to the commercial LiFePO4/C cathode material reference. SEM images show that the particles are of micron size having polyhedral shape. The highest capacity was achieved by LFP/C with 30% carbon addition and excellent cycle and rate performance which exceeds the rate performance of commercial LiFePO4 due to the successful formation of carbon coatings on the LiFePO4 particles. The EIS test shows that LFP with 30% carbon addition has the highest ionic conductivity compared to other samples. It can be concluded that producing LiFePO4 from pretreated poor grade raw material using rheological route can be considered promising to be adapted for mass production.

Acknowledgment

This study is supported by Indonesia Endowment Fund for Education (LPDP/Lembaga Pengelola Dana Pendidikan) through Pendanaan Riset Inovatif Produk (Rispro) Invitasi grant no. PRJ-6/LPDP/2020.

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Received: 2020-09-25
Revised: 2021-03-18
Accepted: 2021-04-07
Published Online: 2021-05-05

© 2021 Meidiana Arinawati et al., published by De Gruyter

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

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  86. Prediction of the parameters and the hot open die elongation forging process on an 80 MN hydraulic press
  87. Special Issue: AEVEC 2020
  88. Vocational Student's Attitude and Response Towards Experiential Learning in Mechanical Engineering
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  100. A review on the fused deposition modeling (FDM) 3D printing: Filament processing, materials, and printing parameters
  101. Facile rheological route method for LiFePO4/C cathode material production
  102. Mosque design strategy for energy and water saving
  103. Epoxy resins thermosetting for mechanical engineering
  104. Estimating the potential of wind energy resources using Weibull parameters: A case study of the coastline region of Dar es Salaam, Tanzania
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  115. Allocation of risk factors for geodetic tasks in construction schedules
  116. Pedestrian fatality risk as a function of tram impact speed
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  118. Finite element analysis of train speed effect on dynamic response of steel bridge
  119. New approach to analysis of railway track dynamics – Rail head vibrations
  120. Special Issue: Trends in Logistics and Production for the 21st Century - Part I
  121. Design of production lines and logistic flows in production
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  123. Modeling of the two shuttle box system within the internal logistics system using simulation software
  124. Implementation of the logistics train in the intralogistics system: A case study
  125. Assessment of investment in electric buses: A case study of a public transport company
  126. Assessment of a robot base production using CAM programming for the FANUC control system
  127. Proposal for the flow of material and adjustments to the storage system of an external service provider
  128. The use of numerical analysis of the injection process to select the material for the injection molding
  129. Economic aspect of combined transport
  130. Solution of a production process with the application of simulation: A case study
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  133. Utilization of intelligent vehicle units for train set dispatching
  134. Special Issue: ICRTEEC - 2021 - Part I
  135. LVRT enhancement of DFIG-driven wind system using feed-forward neuro-sliding mode control
  136. Special Issue: Automation in Finland 2021 - Part I
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  138. Model predictive control for a multiple injection combustion model
  139. Model-based on-board post-injection control development for marine diesel engine
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https://doi.org/10.1515/eng-2021-0068
Schlagwörter für diesen Artikel
LiFePO4; rheology; composite; synthesis; Li-ion batteries; cathode
Creative Commons
BY 4.0

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  75. Laboratory studies of the influence of the working position of the passenger vehicle air suspension on the vibration comfort of children transported in the child restraint system
  76. Route optimization for city cleaning vehicle
  77. Efficiency of electric vehicle interior heating systems at low ambient temperatures
  78. Model-based imputation of sound level data at thoroughfare using computational intelligence
  79. Research on the combustion process in the Fiat 1.3 Multijet engine fueled with rapeseed methyl esters
  80. Overview of the method and state of hydrogenization of road transport in the world and the resulting development prospects in Poland
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  83. Special Issue: Terotechnology 2019 - Part II
  84. DOE Application for Analysis of Tribological Properties of the Al2O3/IF-WS2 Surface Layers
  85. The effect of the impurities spaces on the quality of structural steel working at variable loads
  86. Prediction of the parameters and the hot open die elongation forging process on an 80 MN hydraulic press
  87. Special Issue: AEVEC 2020
  88. Vocational Student's Attitude and Response Towards Experiential Learning in Mechanical Engineering
  89. Virtual Laboratory to Support a Practical Learning of Micro Power Generation in Indonesian Vocational High Schools
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  92. Car braking effectiveness after adaptation for drivers with motor dysfunctions
  93. Case study: Vocational student’s knowledge and awareness level toward renewable energy in Indonesia
  94. Contribution of collaborative skill toward construction drawing skill for developing vocational course
  95. Special Issue: Annual Engineering and Vocational Education Conference - Part II
  96. Vocational teachers’ perspective toward Technological Pedagogical Vocational Knowledge
  97. Special Issue: ICIMECE 2020 - Part I
  98. Profile of system and product certification as quality infrastructure in Indonesia
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  100. A review on the fused deposition modeling (FDM) 3D printing: Filament processing, materials, and printing parameters
  101. Facile rheological route method for LiFePO4/C cathode material production
  102. Mosque design strategy for energy and water saving
  103. Epoxy resins thermosetting for mechanical engineering
  104. Estimating the potential of wind energy resources using Weibull parameters: A case study of the coastline region of Dar es Salaam, Tanzania
  105. Special Issue: CIRMARE 2020
  106. New trends in visual inspection of buildings and structures: Study for the use of drones
  107. Special Issue: ISERT 2021
  108. Alleviate the contending issues in network operating system courses: Psychomotor and troubleshooting skill development with Raspberry Pi
  109. Special Issue: Actual Trends in Logistics and Industrial Engineering - Part II
  110. The Physical Internet: A means towards achieving global logistics sustainability
  111. Special Issue: Modern Scientific Problems in Civil Engineering - Part I
  112. Construction work cost and duration analysis with the use of agent-based modelling and simulation
  113. Corrosion rate measurement for steel sheets of a fuel tank shell being in service
  114. The influence of external environment on workers on scaffolding illustrated by UTCI
  115. Allocation of risk factors for geodetic tasks in construction schedules
  116. Pedestrian fatality risk as a function of tram impact speed
  117. Technological and organizational problems in the construction of the radiation shielding concrete and suggestions to solve: A case study
  118. Finite element analysis of train speed effect on dynamic response of steel bridge
  119. New approach to analysis of railway track dynamics – Rail head vibrations
  120. Special Issue: Trends in Logistics and Production for the 21st Century - Part I
  121. Design of production lines and logistic flows in production
  122. The planning process of transport tasks for autonomous vans
  123. Modeling of the two shuttle box system within the internal logistics system using simulation software
  124. Implementation of the logistics train in the intralogistics system: A case study
  125. Assessment of investment in electric buses: A case study of a public transport company
  126. Assessment of a robot base production using CAM programming for the FANUC control system
  127. Proposal for the flow of material and adjustments to the storage system of an external service provider
  128. The use of numerical analysis of the injection process to select the material for the injection molding
  129. Economic aspect of combined transport
  130. Solution of a production process with the application of simulation: A case study
  131. Speedometer reliability in regard to road traffic sustainability
  132. Design and construction of a scanning stand for the PU mini-acoustic sensor
  133. Utilization of intelligent vehicle units for train set dispatching
  134. Special Issue: ICRTEEC - 2021 - Part I
  135. LVRT enhancement of DFIG-driven wind system using feed-forward neuro-sliding mode control
  136. Special Issue: Automation in Finland 2021 - Part I
  137. Prediction of future paths of mobile objects using path library
  138. Model predictive control for a multiple injection combustion model
  139. Model-based on-board post-injection control development for marine diesel engine
  140. Intelligent temporal analysis of coronavirus statistical data
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