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Recycling metals from wastes: a novel application of mechanochemistry Quanyin Tan, and Jinhui Li Environ. Sci. Technol., Just Accepted Manuscript • DOI: 10.1021/es506016w • Publication Date (Web): 17 Apr 2015 Downloaded from http://pubs.acs.org on May 3, 2015

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Recycling metals from wastes: a novel application of mechanochemistry

1

2 3

Quanyin Tan a, Jinhui Li a, *

4

a

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Environment, Tsinghua University, Beijing, 100084, China

6

Address:

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Quanyin Tan: Room 813, Sino-Italian Environmental and Energy-efficient Building,

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School of Environment, Tsinghua University, Haidian District, Beijing 100084, China

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([email protected])

State Key Joint Laboratory of Environment Simulation and Pollution Control, School of

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Jinhui Li: Room 805, Sino-Italian Environmental and Energy-efficient Building, School

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of Environment, Tsinghua University, Haidian District, Beijing 100084, China

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([email protected])

13 14

*Corresponding

author:

[email protected]

(Tel:

+86-10-6279

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+86-10-6277 2048, Address: Room 805, Sino-Italian Environmental and Energy-efficient

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Building, School of Environment, Tsinghua University, Haidian District, Beijing 100084,

17

China)

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Fax:

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Recycling metals from wastes: a novel application of mechanochemistry

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Abstract

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Recycling metals from wastes is essential to a resource-efficient economy, and increasing

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attention from researchers has been devoted to this process in recent years, with emphasis on

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mechanochemistry technology. The mechanochemical method can make technically feasible the

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recycling of metals from some specific wastes, such as cathode ray tube (CRT) funnel glass and

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tungsten carbide waste, while significantly improving recycling efficiency. Particle size

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reduction, specific surface area increase, crystalline structure decomposition and bond breakage

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have been identified as the main processes occurring during the mechanochemical operations in

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the studies. The activation energy required decreases and reaction activity increases, after these

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changes with activation progress. This study presents an overall review of the applications of

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mechanochemistry to metal recycling from wastes. The reaction mechanisms, equipment used,

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method procedures, and optimized operating parameters of each case, as well as methods

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enhancing the activation process are discussed in detail. The issues to be addressed and

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perspectives on the future development of mechanochemistry applied for metal recycling are also

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presented.

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Key Words

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Mechanochemistry, metal, recycling, activation, wastes

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1 Introduction

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Mechanochemistry is a branch of chemistry, which the widely accepted definition of it is

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proposed by Heinicke in 1984 1, 2. It focuses on the chemical and physicochemical changes during

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aggregation, induced by the effects of mechanical energy. The processes providing the mechanical

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energy for mechanochemistry include milling, grinding, scratching, polishing, shearing, and rapid

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friction

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connected to new developments in milling technology and equipment. Typically, the equipment

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used for mechanical activation includes the retschmill, tumbling mill, stirring ball mill, vibration

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mill, pin mill, rolling mill, and planetary ball mill.

3, 4

. Equipment plays the key role in mechanochemistry, whose progress is closely

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Recent innovative procedures in mechanochemistry are more environmentally friendly, and

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include many advantages when compared with traditional technological procedures. For example,

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the number of technological stages in the milling process has been decreased by excluding

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operations involving the use of solvents and gases 5, simplifying the process and making it

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possible to obtain metastable products that are difficult or even impossible to obtain with

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conventional methods 6.

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Mechanochemistry has been well established in chemistry and material science 7. Various

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processes take place during the mechanochemical procedure, such as the comminution of particles

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to small size, the generation of new surfaces, point defects and dislocations in crystalline structure,

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and polymorphic transformations8-10. Some chemical reactions, including decomposition,

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oxidation-reduction, ionic exchange, and complex and adduct formation, will occur as well

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Two similar terms—mechanical activation (MA) and mechanochemical activation (MCA)—are

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frequently used in mechanochemistry depending on the effect caused during the activation

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.

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operation. MA involves an increase in the reactivity of target substances 7, while MCA refers to

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the accumulation of defects (amorphization process), the formation of polymorphs and the

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occurrence of chemical reactions 13. Mechanochemistry has been applied in a wide range of fields,

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such as chemical engineering, materials engineering, mineral processing, the coal industry, the

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building industry, pharmacy, agriculture, and extractive metallurgy 14. The field of waste treatment

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has also benefited from mechanochemistry, for instance, removing organic pollutants from the soil,

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waste rubber recycling and fly ash modification 15, 16.

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Metal recycling is an essential component of the goal of closed-loop material systems and

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sustainability17. Although the recycling rate for the "base metals" (iron, aluminum, zinc, copper

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etc.) is above 50%; it is less than 1% for the “rare” metals used for precise technological purposes

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in small quantities, such as indium, lithium, and rare earth elements

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more difficult to separate out. In recent decades, intensive efforts and research have been devoted

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to recycling metals from wastes, such as spent lithium-ion batteries (LIBs)

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tube (CRT) glass 21, waste fluorescent lamps (FLs) 22, catalysts 23, and magnets 24.

18, 19

. These metals are also

20

, scrap cathode ray

Hydrometallurgy is one of the commonly used approaches for metal recycling25,

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, and

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mechanochemistry has demonstrated the ability to significantly modify and enhance that process

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27

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hardly be leached out from wastes. It also can improve the leaching efficiency and enhance the

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yield of the original process. It changes the technical route that the wastes have been treated

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through the introduction of new reactions to obtain a better recycling performance for metals. For

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instance, lead in waste CRT glass could hardly be leached out (90% Pb: 99%, Zr & Ti: >90%, La: about 60%

2.8%

planetary

41

86%

CRT funnel glass

RE Es

1 M H2SO4, room temperature, 1h 1 M H2SO4, room temperature, 1h 1 M H2SO4, room temperature, 1h 1 M H2SO4, room temperature, 1h --

1.2%

planetary stirring

Sourc e

90-95% 10-15% 80% 97-98% (indium pellet)

CRT funnel glass planetary

Leaching condition c

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21,

29,

46, 47

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WM, water, L/S: 10, 2h WM, 10% HCl, L/S: 10, 2h

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51% 44%

10% HCl, L/S: 10 -48%

planetary

phosphors

planetary

DM, 2h WM, water, L/S: 10, 2h WM, 7% H2SO4, L/S: 5, 2h DM, 2h

waste phosphors planetary

DM, 3 times (in mass) of NaOH, 5h

7% H2SO4, L/S: 5 7% H2SO4, L/S: 5 7% H2SO4, L/S: 5

62% 70% 59% Y: about 100%; Eu, La, Ce and Tb: > 80% Y: about 100%, Eu: > 90% Ce, La and Tb: >95%

1 M HCl, L/S: 50, ambient temperature, 1h 3 M H2SO4, L/S: 20, 50 ℃, 4h 3 M H2SO4, L/S: 20, 50 ℃, 4h

Co: 35%, Li: 70% Co: >90%, Li: about 100%

1 M HCl, L/S: 100, ambient temperature, 2h

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Co: 0, Li: about 60% Co: >90%, Li: about 100%

water, L/S: 250, ambient temperature, 1h

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electrode scrap from LIS battery

planetary

LiCo2 powder

planetary

W

WC tool waste

planetary

DM DM, 2 times (in mass) of KMnO4, 15 min

W: 25% W: 100%

1 M NaOH, L/S: 20, ambient temperature, 1h

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Cu

waste PCBs

planetary

DM, 0.5 times (in mass) of S powder, 20 min

88.0%

3 M H2SO4, 30 wt% H2O2, L/L/S: 15:15:1, ambient temperature, 1h

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Au

gold-containing waste

Co & Li

577 578

DM, 0.5 times (in mass) of quartz powder, 4h DM, 30h DM, equal-molar ratio of PVC, 30h

78% stirring

WM, water, L/S: 4, 1h WM, acid thiourea solution, L/S: 4, 1h

98% 99%

a

acid thiourea solution (as mentioned above), L/S: 40; 2h (unactivated), 1.5h (activated in water), 1h (activated in thiourea)

DM – dry milling, WM – wet milling; the time refers to time for milling; b the values in “italics” are the yields of original (unactivated) samples; c “--” means no leaching operation was needed; L/S refers to the liquid-to-solid ratio in mL/g; the time refers to the leaching time.

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The structural decomposition resulting from the milling process makes it easier for the leachant

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to attack the metals, as in the decomposition of CRT funnel glass, ceramic, and ITO containing

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cullet. The yield of Pb from CRT funnel glass increased from a negligible 1.2-2.8% to a more than

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92%, Ti and Zr yields from ceramic increased from 50-60% to more than 90%.

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Meanwhile, the external energy added by the activation can also lead to bond breakage and

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even chemical reaction, which could significantly improve the dissolution and/or leaching

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properties and raise the leaching efficiency of the target metal. For instance, it was confirmed that

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the Pb-O bond in CRT glass could be broken during activation, and the LiCoO2 in batteries and

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the WC in tungsten carbide waste could be transformed to easily leachable LiCl, CoCl2 and

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K2WO4. The reduction in particle size and the increase in specific surface area could also enhance

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the leaching of metals with the progress of activation. These physical and chemical changes after

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activation indicate a decrease in activation energy and an increase in reaction activity, making the

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extraction more likely to occur, in less time.

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The milling operations can also be enhanced with the addition of hard particles as grinding aids, 41

or quartz

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such as Al2O3

. Some solid reactions could be introduced to assist the recycling

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process through dry milling operations with reagents, such as the reduction of indium by Li3N 43,

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oxidation of tungsten by KMnO4

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target metals can also be partially or totally extracted from waste simultaneously with a wet

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milling process, which is designed to carry out the activation and leaching in one step, and can

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achieve the advantages of saving time and simplifying the procedure.

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, and transformation of copper by sulfur

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. What is more,

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Obvious improvements of recycling metals in wastes by mechanochemical methods have been

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validated via practices from the perspective of recycling efficiency. Herein, a brief energy balance

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and economic assessment is conducted to have an insight to the application of mechanochemistry

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to metal recycling from waste from other perspectives, taking the study by Ou and Li91 as a

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specific case. The detailed methodology and data used are presented in the Supporting Information.

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According the energy balance, no more than 44.2% of the electricity consumed during the milling

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process can be effectively used for introducing the reaction, most of the external energy is

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transformed into heat, mechanical energy of equipment etc. A revenue of approximately 43.44

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CNY (49.27 CNY after further optimization) can be obtained from the copper sulfate recovered

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(for recycling 1 kg enriched samples). This value can cover the cost (39.67 CNY) of this approach

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when the cost of the capital equipment, transporting, or labor etc., is not counted. At the same time,

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the cost also can be reduced through improvements on the energy efficiency and materials

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consumption when the scale is expanded.

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There are still some theoretical issues waiting for further investigation before its industrial

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application. The efficiency of mechanical and mechanochemical activation obtained in studies

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may need further improvement. It is time- and energy-consuming to determine experimentally the

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optimum conditions for mechanochemical processes in practical application, using pilot projects

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and then implementing them on a wide scale in industrial plants.

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The planetary ball mill is the most often used apparatus in the studies. It can generate a

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relatively higher energy density, producing high mechanical and mechanochemical activation in a

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relatively short milling time 101. The pot mill and stirring mill apparatus are the other two types of

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mills used in the studies. However, proper milling apparatus that can generate sufficient rotational

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speed, impact energy essentially, for industrial applications should be developed, considering the

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control of other process parameters, such as temperature and atmosphere.

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Application of mechanochemical methods to recycling metals from various wastes is still

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conducted at the lab scale. More attention needs to be devoted to addressing the difficulty of

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scalability of the mechanochemical operation, as well as predicting the relevant energy

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consumption and outcomes. After that, mechanochemistry technology can be expected to

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significantly contribute and broaden its application to the recycling of metals from wastes, and

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benefits the environment and society.

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Acknowledgments

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This study is financially supported by the National Nature Science Foundation of China

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(21177069) and is also supported by the National Key Technologies R&D Program (NO.

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2014BAC03B04). We would also like to thank Dr. Xianlai Zeng and Dr. Qingbin Song for their

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valuable advices. The authors are also very grateful to Brenda Lopez for reviewing the grammar

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of the manuscript.

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