Effect of Mechanical Alloying in Polymer- Ceramics Composites · Ceramics · Alumina · Polymer...

Effect of Mechanical Alloying in Polymer-Ceramics Composites

M. V. Khumalo and M. C. Khoathane

ContentsIntroduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2Polymer Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3Ceramics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Natural Raw Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6Classification of Ceramic Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

Nanomaterials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8High-Energy Ball Milling (HEBM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

Techniques and Methods of HEBM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10HEBM in Polymer-Ceramics Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

HEBM in Thermoplastic Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11HEBM in Thermoset Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16HEBM in Polymer Metal Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17HEBM in Carbon/Graphite Matrix Composites (CGMC) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

AbstractThe chapter presents polymer-ceramics composites using mechanical alloying(MA). Ceramics are classified as inorganic and nonmetallic materials that areessential to our daily lifestyle. Many ceramics, both oxides and non-oxides, arecurrently produced from polymer precursors. Ceramics generally has an amor-phous or a nanocrystalline structure and has excellent structural stability, oxida-tion resistance, creep resistance, high-temperature mechanical properties, and

M. V. Khumalo (*) · M. C. KhoathaneDepartment of Chemical, Metallurgical and Materials Engineering, Polymer Technology Division,Tshwane University of Technology, Pretoria, South Africae-mail: [email protected]; [email protected]

© Springer Nature Switzerland AG 2019C. M. Hussain, S. Thomas (eds.), Handbook of Polymer and Ceramic Nanotechnology,https://doi.org/10.1007/978-3-030-10614-0_3-1

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good dielectric properties. Nevertheless, they have a fundamental weakness inthat they are easily fractured and require high-temperature processes for thefabrication of integrated substrates. Composites are now one of the most impor-tant classes of engineered materials, because they offer several outstandingproperties as compared to conventional materials. Composites are a fast-devel-oping segment of the polymer industry; composites filled with materials having atleast one dimension in the micro- and nanometer-size range such as nanofillers,nanoclays, or nanotubes and ceramics represent a step change in technology in thecomposite area. MA is a solid-state powder processing technique involvingrepeated welding, fracturing, and rewelding of powder particles in a high-energyball mill. This technique was originally developed to produce oxide dispersion-strengthened (ODS) nickel- and iron-based superalloys for aerospace applica-tions. MA has been substantiated to be capable of synthesizing a variety ofequilibrium and nonequilibrium phases, including nanocrystalline and amor-phous materials. Recently MA has been demonstrated to be the most versatileand economical process for the synthesis of nanocrystalline materials, due to itssimplicity, low cost, and ability to produce large amount of material. The chapterfocuses on the preparation processes; general microstructures; mechanical, chem-ical, electrical, and optical properties; and potential applications.

KeywordsCeramics · Alumina · Polymer composites · Polymer nanocomposites ·Mechanical alloying · Composites · Nanocomposites · Clays · High-energy ballmilling

Introduction

High-performance plastics and composites, which were developed in the twentiethcentury, have penetrated the international economy and people’s lives in differentfields with an exceptional rate of development in the history. They have become thesubstitutes for traditional materials, showing improved performance. Now, with thespeedy development of science and technology, materials play an important role inthe international economy. New materials are still the beginning of new technolo-gies, and materials science, energy technology, and information science havebecome the three pillars of modern science and technology (Wang et al. 2011).The two main kinds of polymers are thermoplastics and thermosets. According toworldwide researches, production of thermoplastics is approximately 200 billionpounds per year or approximately 25 pounds for every person on the planet. Only asmall fraction of this amount is filled and used as a composite, but a small fraction ofthis large number is still a significant amount of material (Thomas et al. 2012). By farthe most important thermoplastic composites are made from flexible thermoplastics,i.e., semicrystalline materials with a glass-transition temperature below room tem-perature. Thermoplastics applications are in flexible and rigid packaging, motorindustry, engineering sector, agriculture, etc. Thermosets are simply melted resins

2 M. V. Khumalo and M. C. Khoathane

that chemically react from low-viscosity liquids to form solid materials duringprocessing, a process called curing. Thermosets are commonly used for high-tem-perature applications; some of the common products are electrical equipment, motorbrush holders, printed circuit boards, circuit breakers, etc. Commercial plastic resinsmay contain two or more polymers in addition to various additives and fillers. Theseare added to improve some properties such as the processability; thermal, chemical,or environmental stability; and mechanical properties of the final products (Sperlingand Sperling 2006; Fried 2014). The term composite materials was first used inabroad in the 1950s, and it has been used domestically from about the 1970s.Composite material is a kind of complex multicomponent multiphase system, andit is difficult to be defined accurately. A composite material is made by combiningtwo or more materials, a unique combination that yields superior properties thatcannot be met by conventional monolithic materials, such as metal and its alloys,ceramics, and polymers (Rayson 1983; Mallick 1993, 2007). The purpose of com-posites is to allow the new materials to have strengths from both materials, fre-quently covering the original materials’ weaknesses. Composites are different fromalloys because they are combined in such a way that it is difficult to tell one particle,element, or substance from the other. They are usually classified by the type ofreinforcements used. The reinforcements are embedded into a matrix that holds ittogether and used to strengthen the composites (Park and Seo 2011). Compositematerials have several advantages over traditional engineering materials, whichmade them more attractive in many industrial applications. Composite materialshave superior mechanical properties and are commonly classified at the followingdistinct two levels: The first level of classification is usually made with respect to thematrix constituent. The major composite classes include organic matrix composites(OMCs), metal matrix composites (MMCs), and ceramic matrix composites(CMCs). The term organic matrix composite is generally assumed to include twoclasses of composites, namely, polymer matrix composites (PMCs) and carbonmatrix composites commonly referred to as carbon-carbon composites. The mostimportant inorganic nonmetallic matrix composite materials are ceramic matrixcomposites (CMCs) and carbon-based composite materials such as C/C compositematerials (Fig. 1).

These four types of matrices produce common types of composites. A majority ofthe composites used commercially are polymer-based matrices. In composite, matrixis an important phase, which is defined as a continuous one. The important functionof a matrix is to hold the reinforcement phase in its embedded place, which acts asstress transfer points between the reinforcement and matrix and protects the rein-forcement from adverse conditions (Clyne 1996).

Polymer Matrix Composites

Polymer matrix composites (PMCs), because of their inherent characteristics, havebecome the fastest growing and most widely used composite materials. Comparedwith traditional materials such as metals, PMCs have the following characteristics:

Effect of Mechanical Alloying in Polymer-Ceramics Composites 3

• High specific strength and modulus• Excellent fatigue and fracture resistance• Good damping characteristics• Multifunctional performance• Good processing techniques• Anisotropic and property designability• High fracture toughness• Good puncture resistance• Good corrosion and abrasion resistance• Low cost• Lower thermal expansion properties

PMC consists of thermoset or thermoplastic matrix resins reinforced by ceramic,metal, fibers, carbon, and graphite that are much stronger and stiffer than the matrix.They are attractive because they are lightweight, stronger, and stiffer than theunreinforced polymers or conventional metals. PMC, with the additional advantageof their properties and forms, can be tailored to meet the needs of a specificapplication. High-performance reinforcement materials are of the highest interestin various industries like military and aerospace (Council, N.R. 2005). Basically allcommercially important polymers have applications where the polymer is filled,although definitely some materials are more commonly filled than others. Typically,the reason that a specific polymer is a good or bad candidate for use as thecontinuous phase of a composite is its ability to form strong interactions with aparticular filler. Polymers make ideal materials as they can be processed easily andpossess light weight and desirable mechanical properties. Both thermoset andthermoplastic resins could be used as the polymer phase; the former has theadvantage of low viscosity, while the latter has the advantage of the possibility ofrecycling and reuse (Jawaid and Khan 2018; Gay and Hoa 2007; Mazumdar 2001).The use of polymer composites in various engineering applications had become stateof the art. The multiauthor volume provides a useful summary of updated knowledge

Matrices

MetalMatrix Composites

(MMC)

CeramicMatrix Composites

(PMC)

Carbon andGraphic matrix

composites(CGMC)

Polymer MatrixComposites

(PMC)

Thermosets Thermoplastics

Fig. 1 Classification of matrix materials


on polymer composites in general, practically integrating experimental studies,theoretical analyses, and computational modelling at different scales, i.e., fromnano- to macroscale. Comprehensive consideration was given to four major areas:structure and properties of polymer nanocomposites, characterization and modelling,processing and application of macrocomposites, and mechanical performance ofmacrocomposites. Reinforcement phase is the principal load-carrying member in acomposite. Therefore, the orientation of the reinforcement phase decides the prop-erties of the composite (Strong and Strong 2000).

Ceramics

Overview

Ceramics has been the focus of increased interest during the last century since theyexhibit better hardness, stiffness, and chemical stability compared to many othermaterials. The word ceramics originated from “keramos” meaning burnt stuff and isderived from the Greek word “keramikos.” Ceramics cover a vast area of inorganic,nonmetallic materials including white wares, structural clay products, refractories,glass and glass ceramics, cement, concrete, lime, foundry sand, oxide ceramics, andnon-oxide ceramics such as boride, carbide, and nitride. Developments in thetwentieth century that stimulated progress in ceramics include advances in scienceand technology in general, the rise of new industries, advances in military technol-ogy, and also the overwhelming concern for health, safety, and environment(Kingery 1976; Norton 1974; Ichinose et al. 1987; Noboru 1987; Searle andGrimshaw 1959; Singer 2013; Ramaseshan et al. 2007). Ceramics are generallycategorized as conventional or traditional ceramics which contain clay and clay-based materials and high-tech or advanced ceramics which are from synthetic rawmaterials and have specific structural and functional properties. The highest attrac-tion of structural ceramics has constantly been the capability of operating at tem-peratures far above those of metals. Structural applications include enginecomponents, cutting tools, and chemical process equipment. Electronic applicationsfor ceramics with low coefficient of thermal expansion and high thermal conductiv-ity include superconductors, substrate magnets, and capacitors (Norton 1974)(Table 1).

Many compounds in ceramics contained both ionic and covalent bonding. Thegeneral properties of those materials depend on the dominant bonding mechanism.Compounds that were either mostly ionic or mostly covalent had higher meltingpoints than compounds in which neither kind of bonding predominates. In polymers,the bonding within the chains is covalent (strong and directional), while the hydro-gen bonding and van der Waals forces between the chains are relatively weak; higherthermal expansion coefficients and lower stiffness etc. In ceramics, different types ofbonding mechanism could occur: ionic, e.g., in oxides and silicates (Al2O3, MgO,SiO2, etc.); covalent, e.g., in nonmetallic carbides and nitrides (SiC, B4C, BN, Si3N4,


AlN, Si2N2O, SiO2, etc.); and metallic, e.g., in transition-metal carbides and nitrides,etc., and they often coexist in the same physicochemical phases.

Natural Raw Materials

It has been understood that clay mineral is an excellent raw material for various high-temperature ceramic requirements. The ceramic properties of clays are largelygoverned by the crystal structure and the crystal composition of their essentialconstituents and the nature and amount of accessory minerals present. Since silicatesand alumina silicates are easily available, they are also inexpensive and thus providethe backbone of high tonnage products in ceramic industry (Veniale 1990; Pampuch1976). The principal clay mineral groups are kaolinite, smectite, and palygorskite.Clay minerals can be divided into chain and layer structures. The layer structures arebranched into 1:1 and 2:1 (dimorphic and trimorphic). Classification of clay mineralsis indicated below (Fig. 2).

Classification of Ceramic Matrix Composites

CMCs are a family of new materials which are attracting considerable industrialinterest and investment worldwide. They are defined as materials whose microstruc-tures compromise a continuous metallic phase (the matrix) into which a secondphase, or phases, has been artificially introduced (Feest 1986). CMCs can be dividedinto two types: microcomposites and nanocomposites. In microcomposites, micro-size second phases such as particulate, platelet, whisker, and fiber were dispersed atthe grain boundaries of the matrix. Some of the more common discontinuousreinforcements include whiskers, platelets, and particulates having compositions ofSi3N4, silicon carbide (SiC), aluminum nitride (AlN), titanium diboride, boroncarbide, and boron nitride. Of these, silicon carbide has been the most widely usedbecause of its stability with a broad range of ceramic oxide and non-oxide matrices(Belitskus 1993; Bunsell and Renard 2005). The main purpose of these composites isto improve the fracture toughness. The nanocomposites can be grouped into threetypes: intragranular composites, intergranular composites, and nanocomposites asshown in Fig. 3. As schematically drawn in the figure, in the intra- and intergranularnanocomposites, the nano-size particles are dispersed mainly within the matrix

Table 1 Ceramics variety of chemical bonding

Compound Melting point �C Covalent % Ionic %

MgO 2798 27 73

Al2O3 2050 37 63

SiO2 1715 49 51

Si3N4 1900 70 30

SiC 2830 89 11


grains or at the grain boundaries of the matrix, respectively. Their aim is to improvenot only the mechanical properties such as hardness, fracture strength and toughness,and reliability at room temperature but also high-temperature mechanical propertiessuch as hardness strength and creep and fatigue fracture resistances (Mohanty et al.2016; Sternitzke et al. 1997).

CMCs are one of the promising materials; by combining different ceramic matrixmaterials with special suitable fibers, new properties can be created and tailored forinteresting technical fields (Lee 1992; Clauss and Schawaller 2006; Wang et al.2010). CMCs were established to overcome the intrinsic brittleness and lack ofreliability of monolithic ceramics, with a view to introduce ceramics in structuralparts used in severe environments, such as rocket and jet engines, gas turbines forpower plants, heat shields for space vehicles, fusion reactor first wall, and heattreatment furnaces (Sternitzke 1997). Ceramic matrices could be characterized aseither oxides or non-oxides and in some cases might contain residual metal afterprocessing (Laurent et al. 1994; Breval et al. 1985). Some of the more commonoxide matrix includes alumina, silica, and mullite. Alumina have been the mostwidely used because of their in-service thermal and chemical stability and theircompatibility with common reinforcements.

Three layer type(2:1)

Two layer type(1:1) Chain structure typeRegular mixed layer

type

Layer Structure

(Sheet structure

composed of one

silica layer and one

alumina layer)

(Sheet structure

composed of two silica

layers and one alumina

layer)

(Ordered stacking of

alternate layers of

different types e.g.

Chlorite group)

(Hornblende like

chains) e.g. Attapulgite,

sepiolite palygorskite

Equi dimensional (Kaoline group)

Elongate (Halloysite group)

Equi dimensional (montmorillonite

group)

Elongate(montmorillonite

group)

e.g.

Montmorillonite,

Nontronite saponite,

hectorite

e.g. Montmorillonite

vermiculite, sauconite

e.g Halloysitee.g. Kaolinite,

Dickite Nacrite etc

Fig. 2 The category of layer structure steps for natural raw materials


Nanomaterials

Nanostructured (NS) materials are defined as solids having microstructural featuresin the range of 1–100 nm (= (1–100) � 10–9 m) in at least one dimension(Balasubramanian 2013). These materials have outstanding mechanical and physicalproperties due to their extremely fine-grain size and high grain boundary volumefraction. When the size of material is in the range of nano-size, the main componentsof the material concentrate on the surface. For example, when the particle is 2 nm indiameter, the surface atoms will occupy 80% overall. The enormous surface couldproduce surface energy, and then nanometer-sized objects generate the strongaggregation, which enlarges the particle size. Ceramics-based nanocomposites andmetal-based nanocomposites can be made by the method of nano-phase in situgrowth; their performances were improved significantly, but there are still difficultiesin accurately controlling the content of reinforcements and the chemical compositionof generated products by in situ reaction. Organic-inorganic molecular interactionshave covalent bond type, coordination bond type, and ionic bond type; each type ofnanocomposite material has its corresponding preparation methods. For example,the preparation of nanocomposites with covalent bond type adopts the sol-gelmethod basically. The material can achieve the level of the dispersion of moleculargrade, so they get the superior performance (Wang et al. 2011). High-energymechanical milling can be used to produce nanopowder. There are two routes forproducing nanopowders using mechanical milling: (a) milling a single-phase powderand controlling the balance point between fracturing and cold welding, so that

Fig. 3 The classification ofceramics nanocomposites(Niihara 1991)


particles larger than 100 nm will not be excessively cold welded, and (b) producingnanopowders using mechanochemical processes (Zhang 2004).

High-Energy Ball Milling (HEBM)

A new process called “mechanical alloying” (MA) had been developed, whichproduces homogeneous composite particles with an intimately dispersed, uniforminternal structure. Materials formed by hot consolidation of the powders achieved thelong-sought-after combination of dispersion strengthening and age hardening in ahigh-temperature alloy. Mechanical milling (involving one material) and mechanicalalloying (involving two or more materials) are generally referred to as high-energyball-milling techniques employed to process materials in the solid state. Thosenonequilibrium processing routes responsible for the early successes in oxide dis-persion strengthening of metallic superalloys involve a variety of metastable inor-ganic materials. The morphologies (both single component and alloys) are used toform extended solid solutions, novel intermediate phases, alloys from immisciblemetals and oxides, metal-ceramic composites, and nanocrystalline materials (Kochand Whittenberger 1996; Lü and Lai 2013; Murty and Ranganathan 1998; Benjamin1970). Since its inception by Benjamin around 1966, HEBM has been used toproduce oxide dispersion-strengthened (ODS) iron- and nickel-based alloys foraerospace engineering. Mechanical alloying (attrition, also generally known asHEBM) was a multipurpose tool to produce nanostructured materials with a widevariety of chemical compositions and atomic structures (Budin et al. 2009). Thematerial/particle dimension did not matter significantly, as long as it was smaller thanthe size of the balls, because material is grinded within a very short period of timeand becomes powder with the high energy impact of the balls (Gupta et al. 2017).Ball milling can enable the purposeful execution of physical and chemical trans-formations in powdered materials.

That method confirmed that the physical and chemical behaviors of moleculesand ordered and disordered solids could be affected by non-hydrostatic mechanicalstresses and the associated strains (Delogu et al. 2017). Ball milling was performedat room temperature on dry mixtures of powders, which had the undisputableadvantages of avoiding the need for high temperatures, hazardous solvents, andcomplex in situ polymerization processes. In addition, ball milling not onlyrepresented an interested alternative for the mass production of hybrid organic-inorganic materials; it is also an environmentally and economically sustainablemethod for fabricating nanocomposites with temperature-sensitive molecules.

For the past two decades, HEBM has broadly been used as a versatile process toproduce a variability of progressive compound powders. The core differencebetween high-energy milling by planetary ball mill, Spex mill, Attritor mill, etc.and conventional milling was that the previous method applied considerably largerdoses of energy to the particles over time. Significant improvement in mechanical,chemical, and physical properties have been achieved, through chemistry modifica-tions and conventional thermal, mechanical, and thermomechanical processing


methods (Suryanarayana 2001; Baláž et al. 2013; Takacs 2002). The large amount ofenergy consumed by high-energy mills was possibly a burden in its industrialapplication of the method. That was because the electrical energy consumed forthe production of the powders by high-energy mills was added to the final price ofthe products (Fernandez-Bertran 1999). Scientific investigations by materials scien-tists have been directed continuously toward improving the properties and perfor-mance of materials (Table 2).

Techniques and Methods of HEBM

Ball milling has been applied in numerous solvent-free carbon-carbon bond forma-tions. Various types of ball mills are known, and they include ball mills (drum), jetmills, bead mills, vibration ball mills, planetary ball mills, and horizontal rotary ballmills (M’Hamed and Alduaij 2016). All of these devices are based on the principlethat a starting material is placed between two surfaces and crushed because of theimpact and/or frictional forces that are caused by collisions between these surfaces.The various mills differ in the method of how the motion causes the collisionscreated. Besides the intensive grinding effect, the collisions often lead to an energytransfer, which results in an increase of internal temperature and pressure. For theachievement of better control of these factors, some ball mills have cooling/heatingdevices attached. In general, ball mills are able to produce materials with a particlesize of �100 nm. Rodriguez et al. described a planetary ball mill that contained amain disk that can rotate at a high rotational speed and can accommodate one to eightgrinding bowls. These bowls hold a number of balls as grinding medium and rotatearound their own axes in opposite directions, relative to the main disk. The rotationalspeeds are between 100 and 1000 rpm. Vibration ball mills contain only one or twogrinding chambers, which accommodate one or more grinding balls, and can beshaken at a frequency of between 10 and 60 Hz in three orthogonal directions. Somevibration ball mills have cooling/heating systems, which allow temperature controlwhile grinding (Rodriguez et al. 2007).

Other terms found in the literature to describe the same milling technique arehigh-speed ball milling (HSM), high-speed vibrational ball milling (HSVM), shakermilling, and HEBM. Horizontal rotary ball mills have the advantage that they couldbe operated at a high relative velocity of the grinding medium (up to 14 ms�1) thatcannot be reached by other types (up to 5 ms�1) (Lin and Nadiv 1979).

The HEBM media are comprised of the milling balls, grinding vessel, vial, jar,and bowl. The HEBM media are a major source of contamination via diffusion aswell as abrasion. Stainless steel, hardened steel, tungsten carbide (WC), and zirconia(ZrO2) are the most commonly used HEBM media. Often, process-controllingagents (PCA) are used to decrease the sticking of powder to the balls and walls ofthe milling jar. PCA can be in solid, liquid, or gaseous form and can get adsorbed onthe surface of the metal, thereby causing a reduction in surface energy. The millingtemperature is an important variable (Gupta et al. 2017). For high-temperaturerequirements, electrically heating is employed to heat the milling vial in order to


increase the temperature of milling, and this is expected to promote alloying processthrough diffusion. This can lead to an increase in the minimum achievable grain size.Milling speed was varied depending on the type of ball mill, ball-to-powder ratio,and purpose of HEBM. A higher milling speed which led to higher impact energycaused faster grain refinement (Mio et al. 2002, 2004). Aluminum (A‘) is a reactiveelement; therefore milling was performed in an inert atmosphere or in a vacuum.Argon (Ar) was the most commonly used milling atmosphere. Use of nitrogen,hydrogen, and helium was also reported. Other gases, i.e., NH3, could be introducedto induce chemical reactions, which led to reactive HEBM. Ball-to-powder weightratio (BPR) had significant effect on the kinetics of alloying and/or grain refinement.BPR largely depended on the purpose and type of HEBM. A small BPR might notinduce any significant grain refinement. Milling time is a very important factor,which should be long enough to achieve steady-state grain reduction and completealloying. However, longer ball-milling time increases the chances of contaminationand costs time and money and might led to the formation of unwanted phases(Suryanarayana 2001) (Fig. 4).

HEBM in Polymer-Ceramics Composites

HEBM is one of the effective processes for fabricating polymer-ceramic compositepowders as it allows incorporation of the ceramic phases into the polymer particles.The technique of polymer nanocomposites with nano-sized ceramic particulatereinforcement can be produced through numerous deformations, fracturing, andcold welding events. After a certain period of milling, powder microstructurehomogeneity can be achieved. The simplicity, high efficiency, and low cost ofball-milling method have attracted scientists’ attention (Tadayyon et al. 2011).Alumina is a ceramic metal oxide of great importance. The material was used asbuilding material, refractory material, and electrical and heat insulator, due to its highstrength, corrosion resistance, chemical stability, low thermal conductivity, and goodelectrical insulation (Huang et al. 2003).

HEBM in Thermoplastic Matrix Composites

Medium-density polyethylene (MDPE) powder reinforced with nano-sized alumina(Al2O3) particles. SEM of pure MDPE regular shape powder converted to the flake

Table 2 Typical capacities of the different types of mills (Suryanarayana 2001)

Mill type Sample weight

Mixer mills Up to 2 � 20 g

Planetary mills Up to 4 � 250 g

Attritors 0.5 to 100 kg

Uni-ball mill Up to 4 � 2000 g


shapes as milling time increased. The demonstrated that an increase in milling timecauses the agglomeration of alumina to decrease. The DSC profiles of samplesexplained that ball milling has little effect on crystalline temperature and meltingpoint of all materials including MDPE and its nanocomposites. The nanocompositeshows more thermal stability than pure polyethylene as proven by TGA tests(Tadayyon et al. 2011; Ma et al. 2002). During the HEBM process, the outcomesshowed that the consistent shape of PBT powders was converted into flakes and thenano-antimony oxide (Sb2O3) particles were well deagglomerated and better dis-persed in the poly(butylene terephthalate) (PBT) matrix. Mechanochemical stimu-lation that was provided by the HEBM process produced a reduction in themolecular weight of PBT, which in favors the first step of thermal degradation.Furthermore, two Tgs were attained in the case of the nanocomposite powders whenthe milling time was over 3 hours, one of them being slightly higher than that of thepure PBT, which showed that there was a special interaction between PBT and nano-Sb2O3 particles. However, the HEBM process led to a decrease of the PBT crystal-linity (Yang et al. 2018, 2019). The authors further explained (PBT) nanocompositescontained modified nano-Sb2O3 particles were dispersed by two different dispersingtechniques, included high speed rotating to disperse (HSR) and high-energy ballmilling to disperse (HEBM). The dispersion, interfacial interaction, and mechanicalproperties of nanocomposites were investigated. The results showed that the disper-sion and compatibility of nanocomposites dispersed by HEBM were better than thatof HSR. From the analysis of interfacial interactions between nano-Sb2O3 particlesand PBT matrix, the interfacial adhesion (B) and tensile strength of interfacial (σi)were decreased with the increase of nano-Sb2O3 particle content.

Polymer-clay nanocomposites were fabricated from medium-density polyethyl-ene and organically modified Na-montmorillonite (MMT) using the planetary ballmilling as a new method. The milling time and the addition of clay have not affectedthe crystal structure of MDPE matrix. The addition of clay reduces the crystallinesize of MDPE. Ball milling was also effective in reducing the crystallite size ofMDPE. The ball milling has influence on the crystallinity of MDPE, especiallyduring the early stage of milling. The crystallinity of MDPE decreases as the claycontents increased. It could reduce the intensity of XRD peaks by only 5 wt% clay(Abareshi et al. 2009). The effect of HEBM under different conditions on thestructure of Na+-montmorillonite (Na-MMT) and the organo-montmorillonite

Fig. 4 Schematic representation of formation of nanocrystalline grains during HEBM (Gupta et al.2017).


(Cloisite 30B) was investigated. Ball milling increased the structural disorder:peeling off of layers from the particles were observed, followed by the exfoliationof the particles, indicated by the disappearance of the (001) reflection (Ramadan etal. 2010). (Wang et al. 2008) reported a novel technology, solid-state shear milling(S3M), to prepare poly(ethylene terephthalate)/Na+-montmorillonite nano-composites used the pristine Na+-MMT without organic modification so as toavoid the problem that the organic modifiers. The intercalated PET/Na+-MMT co-powders could be formed under the strong shear forces of pan milling, increasedinterlayer spacing of pristine Na+-MMT from 1.17 nm to 1.48 nm, which could befurther delaminated during subsequent twin-screw extrusion. The Na+-MMT had aheterogeneous nucleation effected on the crystallization of PET, which was strength-ened by milling. Na+-MMT was incorporated into a poly(e-caprolactone)-starchblend by means of a ball mill. The milling time strongly influenced the mechanicaland barrier properties. In particular, the best results in terms of elastic modulus andpermeability coefficient were achieved with a complete delamination of the pristineclay structure. In summary, the milling process not only had demonstrated to be apromising compatibilization method for immiscible PCL-starch blends, but it couldbe also used to improve the dispersion of nanoparticles into the polymer blends(Vertuccio et al. 2009). Planetary ball mill was employed to produce MDPE matrixnanocomposites reinforced with different clay contents. The results showed theeffects of milling time and clay content on the particle size of polyethylene powder.The results showed that during milling, the regular shape of pure polyethylenepowder converts into flake shapes and the average particle size of the powderincreased upon increasing the milling time because the welding mechanism waspredominant (Abareshi et al. 2010). The potential of ball milling was investigated inthe melt processing of PP-/clay-based compounds to improve the clay dispersion(Perrin-Sarazin et al. 2009). Depending on the milling parameters, the nature of theclay, and the presence of other components during milling, different changes in theclay structure, such as delamination and breakage, have been observed. Neverthe-less, the main concern was the particle agglomeration caused by milling. Preliminarymilling of clay alone led to large particle agglomeration in the case of the organoclay,resulting in poor clay dispersion in the final compounds. Ball milling demonstratedsome potential to improve the dispersion of the clay, especially in the case of theinorganic clays, which could be an alternative to the use of organoclays.

Based on author’s paper, PP/organophilic montmorillonite (OMMT) nano-composites were successfully prepared without any compatibilizers by solid-stateshear compounding (S3C) using pan-mill equipment. When OMMTand PP were co-milled, exfoliation of the OMMT layers as well as formation of nanocomposites ofOMMT with PP could be realized as a result of the weak interlayer structure ofOMMT and the fairly strong shear forces offered by pan milling (Shao et al. 2005).Water-soluble PVP/MMT nanocomposites prepared via solution intercalationmethod were investigated. The nanocomposites prepared by attrition ball millingshowed better optical transparency than the ones by simple stirring because the morerigorous mixing could induce the smaller sizes of tactoid or primary particle in thenanocomposites. PVP and MMT were considerably compatible enough to form an


exfoliated nanocomposite up to 20 wt% MMT contents (Koo et al. 2003). The solid-state shear pan milling was employed to prepare a series of polymer/layered silicate(PLS) nanocomposites. During the process of pan milling at ambient temperature,poly(vinyl alcohol)/organic montmorillonite (PVA/OMMT) was effectively pulver-ized, resulting in coexistence of intercalated and exfoliated OMMT layers. Micros-copy analysis indicated that OMMT dispersed homogeneously in PVA matrix, anddiffraction analysis illustrated that pan milling has an obvious effect on increased inthe interlayer structure of OMMT and resulted in coexistence of intercalated andexfoliated OMMT layers formed (Li et al. 2010). (Sorrentino et al. 2005) investi-gated HEBM used to prepare the composites of poly(3-caprolactone) and modifiedMg-A‘ layered double hydroxide, at different inorganic contents, has a number ofmechanical and physical properties enhanced in comparison with those of the purePCL polymer. The modulus and stress at yield point improved for all the composites,in spite of the molecular weight reduction of PCL. Strain at break point and stress atbreak values improved in the composite sample containing 1.4 wt% of inorganicfiller. The use of solid-state ball milling (SSBM) for dispersed cellulose nano-whiskers (CNWs) in starch-based thermoplastics. Different testings demonstratedstrong correlation between mechanical reinforcement and nanowhisker dispersion(Moreira et al. 2012). The starch-pectin-CNW nanocomposites showed high disper-sion of the nano-sized filler in the matrix; thus SSBM showed great potential whencompared to sol-gel, casting/evaporation, and other methods to disperse thosepromised nanoparticles. Nano-sized boron nitride (BN) powder was successfullyprepared by pulverizing micro-sized BN powder using a ball mill process withoutany wetting agents. In order to enhance the dispersivity of nano-BN in the polymermatrix, the surfaces of the nanoparticles were treated with LDPE, which dissolved inthe cyclohexane solvent. In their investigation, the preparation of nano-sized BN-dispersed HDPE was successfully performed by using an organic solvent surfacetreatment method together with a polymer melt mixing process, and the highlyenhanced thermal conductive characteristics for the nano-BN/HDPE compositeswere observed (Jung et al. 2010). The authors explained the effect of silica nano-particles on structure and morphology of LDPE which was investigated. SiO2

nanoparticles were dispersed in a LDPE with cryogenic HEBM. Although HEBMpromoted the formation of the metastable monoclinic phase in the LDPE, nano-composites in the form of films never showed important differences in their thermaland morphological characteristics, suggesting that there were no high interactionsbetween the polar nanoparticles and the nonpolar polymer and that thermal treatmentwas enough to eliminate the specific microstructure induced by HEBM (Olmos et al.2012). According to the studies, PET/SiO2 nanostructure was induced bycryomilling for 10 h. PET flakes dispersed with single SiO2 nanoparticles formedthe primary composite particles, and conglomerations of those primary compositeparticles were the secondary composite particles (Zhu et al. 2006a). The typical sizesof single SiO2 nanoparticles, PET/SiO2 primary composite particles, and secondarycomposite particles were 30, 400, and 7.6 μm, respectively. The dispersion homo-geneity of SiO2 nanoparticles in PET matrix was far more beyond the capability ofconventional methods, which was ascribed to solid processing, high mechanical


energy of ball milling, and cryogenic temperature. It was realized from the studiesthat ball milling and mixing with strong shear force and strike force were applied toget fine dispersion of nano-SiOx particles in poly(phenylene sulfide) (PPS) powder.Ball milling increased the total systematic interface energy. The bonds allowed SiOxto dissipate and transfer energy and thus improve PPS impact strength from theaddition of nano-SiOx. Crystallization behavior (Tc, Tm, ΔT, Xc, etc.) of nano-SiOx/PPS was influenced by ball milling. Consequently, crystallinity of nano-SiOx/PPSwas reduced by 25%, and its Izod impact strength was increased by 89% (Lu and Pan2006).

Fumed silica nanoparticles with 14 nm of diameter were blended with PMMA, bymeans of a HEBM process. It was demonstrated how to obtain fumed silica-PMMAnanocomposites with a very homogeneous dispersion of the nanoparticles within thePMMA. It has been observed that the properties of the composite were highlydependent on the active milling time: (i) the size of the silica-PMMA nanocompositeparticles decreased, and (ii) the Tg also decreased. The later result has been assignedto a reduction in the molecular weight of the PMMA due to chain scission during thehigh-energy blending process (Castrillo et al. 2007; González-Benito and González-Gaitano 2008). It was further reported by Gonzalez-Benito and his co-worker. Thepresence of silica nanoparticles in the structure, dynamics, and thermos degradationof PMMA. HEBM was used to uniformly disperse nanoparticles within a polymericmatrix (PMMA). FTIR indicated that no signal of degradation processes or second-ary reactions induced by HEBM were observed, as well as no existence of specificinteraction between the silica nanoparticles and the PMMA polymer (Pantaleón andGonzález-Benito 2010). HEBM used co-milling in a solid state by low-temperatureMA to prepare nickel-ferrite (NiFe2O4) nanopowders, ultrafine PMMA, dispersednanoparticles in a polymer matrix, and a uniaxial high-velocity cold compactionprocessed employed a cylindrical, hardened steel die and a new technique withrelaxation assisted has been studied. It was found that a longer mixing time gave ahigher degree of dispersion of the nanopowder on the PMMA particle surfaces(Agyei-Tuffour et al. 2014). Their work demonstrated PEEK/SiO2 nanocompositepowder was successfully produced by HEBM under ambient temperature. Mechan-ical milling led to the deterioration of PEEK crystallites and decreased the degree ofcrystallinity. Mechanical milling has major effects on thermal behavior of PEEK.Nonequilibrium order imposed on the material by repetitive deformation duringmilling might be responsible for the observed changes (Hedayati et al. 2011;Zhang et al. 2008). The development of HEBM and the presence of TiO2 nano-particles on the non-isothermal crystallization and fusion behavior of the HDPEwere investigated. It has been demonstrated that HEBM was a good method toprepare nanocomposites of well-dispersed TiO2 nanoparticles within an HDPEmatrix. It was observed that although in general there was a reduction of crystallinityof the polymer, when nanoparticles were absent, the HEBM process induced adouble crystallization process (appearance of both the orthorhombic and metastablemonoclinic phases) (Olmos et al. 2009). The authors further explained that HEBMpromotes the formation of the metastable monoclinic phase in the LDPE; nano-composites in the form of films did not show important differences in their thermal


and morphological characteristics, suggesting that there are no high interactionsbetween the polar nanoparticles and the nonpolar polymer and that thermal treatmentwas enough to eliminate the specific microstructure induced by HEBM (Olmos et al.2012, 2015). The mechanical properties and morphologies of PP composites filledwith four different sizes of calcium carbonate (CC) particles were studied. It wasclear that the PP matrix and filler size have key effects on improvement of mechan-ical properties of PP matrix. For all three PP matrices, the yield strength, the flexuralstrength, and modulus of composites filled with CC25, CC4, and CC1.8 could beregarded as the same. And the yield strength, the flexural strength, and modulus ofcomposites filled with CC0.07 were obviously lower than those of composites filledwith other sizes of particles. For all particles, the flexural strength and modulus of thecomposites increased with increasing filler content, while the yield strengthdecreased with increasing filler content (Yang et al. 2006). “Al”/PMMA compositeswith low coefficients of thermal expansion were prepared by attritor milling of “Al”and PMMA powders and then hot-pressing the powder mixture. The resistivitydrops by about 10 orders of magnitude as “Al” content was increased from 20 to40 vol %. The attritor milling helps in reducing the critical volume fraction of metalparticles by increasing the aspect ratio. The dielectric constant and dissipation factorof the “Al”/PMMA composites increase with increasing aluminum content, which isdue to interfacial polarization (Singh et al. 1996).

HEBM in Thermoset Matrix Composites

According to Huang (Huang et al. 2012), UV-curable ammonium salt [2-(methacryloyloxy)ethyl]trimethylammonium methyl sulfate (MAOTMA)-modifiedMMT/epoxy nanocomposite samples were prepared with the aid of planetarymechanical milling process. TEM microscopy revealed a uniform dispersion ofexfoliated MMT lamella in epoxy matrix, and the thermal analyses indicated asubstantial improvement on thermal properties, e.g., thermal stability and CTE, ofnanocomposites. Analytical results illustrated that the planetary mechanical millingprocess adopted was a valuable tool for microstructure refinement and physicalproperty enhancement of nanocomposite samples. The induce MMT exfoliatedand homogeneously dispersed in epoxy matrix (diglycidyl ether of bisphenol A)curing in the presence of diaminodiphenyl sulfone and obtained improved mechan-ical properties, a promised new method had been developed to prepare highlyreinforced epoxy/MMT nanocomposites through exerting shearing force on epoxy/MMT solution. When the novel-structured MMTII was sheared by ball milling inketone/epoxy solution during the processing of novel structured epoxy/MMTIInanocomposites, a desirable exfoliation could be achieved in comparison with noball-milling step. The resultant nanocomposites have a high impact toughness, andthe impact strength could be increased up to 48.1 kJm�2 from 32.1 kJm�2, whichwas about 50% higher than that of pristine matrix by ball milling. Modifying agents,being combined with dodecylbenzyldimethylammonium chloride and meta-


xylylenediamine, were used to organically modify the clay (MMTII) (Lu et al.2004).

HEBM in Polymer Metal Matrix Composites

Acrylonitrile-butadiene-styrene (ABS)/iron nanocomposites have been prepared bycryomilling (HEBM under cryogenic temperature), and a microstructure of ironnetwork in ABS matrix was obtained. ABS/Fe nanocomposites have been success-fully obtained by cryomilling. The cryogenic temperature and cryomilling greatlyenhance the size reduction by improving fracture and restricting cold welding. Bothparticles and grains were refined with much faster speed rate, and the comminutionlimited was move to the finer end inaccessible to ambi-milling process. Twentyhours cryomilling pulverizes the single ABS/Fe composite particle smaller than100 nm and refined Fe grains about 20 nm (Zhu et al. 2006b). The authors furtherexplained PANI/iron nanocomposites with both conducting and magnetic propertieshave been prepared by cryomilling (HEBM under cryogenic temperature), in whichthe average size of iron grains attains 20 nm. After cryomilling for 20 h, the averagesize of Fe grains was refined to 20 nm; besides, many of Fe particles were dispersedin PANI matrix. It only needed to take 2 or 5 h to get them dispersed homogeneouslyin the PANI matrix (Zhu et al. 2006c, 2008), but the conductivity decreases graduallywith the cryomilling time after 2 h due to the dedoping of DBSA from PANI matrix.Pan-milling technique was developed to prepare ultrafine PP/Fe composite powders,in which the average grain size of the iron particles attained a nanoscale level. Anaverage grain size of iron below 100 nm was obtained and reached 28 nm after 30milling cycles while co-milling with PP. The experimental results showed that co-milling benefited the size reduction for both PP and iron (Lu and Wang 2004).Microstructural and phase transformation of magnetite induced by HEBM andinfluenced conducted polyaniline (PANI) on Fe3O4 particles was investigated.Through diffraction analysis, it was found that after HEBM, the crystallite size ofFe3O4 particles was rapidly reduced to about 21 nm. Broken PANI chains reactedwith the Fe atoms in the surface of Fe3O4 particles and formed some paramagneticphase and a small number of super paramagnetic α-Fe2O3 particles. The magneticproperties of the composites were also changed (Bao and Jiang 2005). Ethylenevinyl acetate (EVA) copolymer, a thermoplastic semicrystalline polymer, has beenblended with barium titanate submicrometric particles (BaTiO3) by means of HEBMto obtain composites in the form of films by hot-pressing. Two different millingconditions have been considered: room temperature and cryomilling. The character-ization of the samples as powders and films showed the lack of strong interactionsbetween the matrix and the BaTiO3 and that the cryogenic conditions were the mostsuitable to achieve a uniform dispersion of the nanofiller without altering thestructural and morphological properties of the base materials (Serra-Gómez et al.2012; Russell et al. 1997). Magnetic nanocomposites, composed of cobalt ferrite(CoFe2O4) nanoparticles and polyvinyl alcohol (PVA) polymer, were obtained usinga two-step mechanical milling, and the effects of milling time and polymer content


were investigated. It was found that single-phase cobalt ferrite of 20 � 4 nm particlesize is distributed uniformly by increasing PVA amount and milling time up to 80 wt.% and 30 hours, respectively; however, the size and shape of particles were notchanged drastically. The interaction of PVA chains and magnetic phase has beenconfirmed in nanocomposite samples. The obtained results in their work prove thatmechanical alloying could be an efficient way to yield such advanced functionalmagnetic nanocomposites (Rashidi and Ataie 2016). The structural morphological,dielectric, and magnetic properties of CoFe2O4 and various PS concentrations addedwith CoFe2O4 nanoparticles prepared by coprecipitation method were studied(Vadivel et al. 2017). Characterization results indicated that the addition of PS inCoFe2O4 nanoparticles remarkably modified the size of the prepared nanoparticles.Structural analysis by XRD confirms the formation of single-phase cubic spinelstructure, and vibrational spectral analysis confirms the Fe-O symmetrical stretchingvibrational mode. Hence, from the obtained overall results, it could be concludedthat the addition of PS in CoFe2O4 nanoparticles controlled the size of the particlesand thus enhanced the dielectric and magnetic properties of CoFe2O4 nanoparticleswhich would be useful for high-frequency and data storage applications. A polymernanocomposite of nanocrystalline nickel ferrite and polyethylene (PE) was success-fully synthesized using the ball-milling process (Nathani et al. 2004). The ball-milling process did not significantly influence the crystallite size of nanocrystallinenickel ferrite in the composite. Magnetic measurements carried out at room temper-ature suggested characteristics of super paramagnetism, i.e., absence of hysteresis,remanence and coercivity, and lack of saturation magnetization. The nickel ferrite-polyethylene nanocomposite exhibited a blocking temperature of�20 K. The lack ofsaturation magnetization at high field occurs in association with high field irrevers-ibility and open loop at 50. Rashidi and Ataie (Rashidi and Ataie 2015) reported thatmagnetic nanocomposites composed of mixed cobalt ferrite nanoparticles and PVAor polyethylene glycol (PEG) polymer were synthesized using a two-step mechan-ical alloying method. PEG could not undergo the restricted temperature risen andinduced heat during milling process melt in both moderate and slow milling condi-tions. Although cobalt ferrite nanoparticles embedded entirely in melted polymermatrix, and after the initial hours of milling, the obtained composite changes to bulkin ball mill. PVAwas properly mixed with cobalt ferrite particles, and the dispersionof particles with interaction between polymer chains and cobalt ferrite nanoparticleswas obtained in moderate milling condition. HEBM using solid state by low-temperature mechanical alloying to prepare nickel-ferrite (NiFe2O4) nanopowdersand ultrafine poly-(methyl methacrylate) (PMMA), dispersing nanoparticles in apolymer matrix, and a uniaxial high-velocity cold compaction process used acylindrical, hardened steel die and a new technique with relaxation assists hasbeen studied. Experimental results for different milling systems that were presentedshowed the effects of milling time and material ratio. It was found that a longermixing time gives a higher degree of dispersion of the nanopowder on the PMMAparticle surfaces. Furthermore, with increasing content of NiFe2O4 nanopowder, thereduction of the particle size was more effective. Different post-compacting profiles,i.e., different energy distributions between the upper and lower parts of the


compacted powder bed, led to different movements of the various particles andparticle layers. Uniformity, homogeneity, and densification on the surfaces in thecompacted powder are influenced by the post-compacting magnitude and direction(Azhdar et al. 2008; Gotoh et al. 2000). Raju andMurthy (2013) explained a series ofnanocomposites of nickel-zinc ferrite plus paraformaldehyde which was success-fully synthesized using the mechanical milling process. The milling process signif-icantly influenced the crystallite size of nanocrystalline nickel-zinc ferrite in thecomposite. With the increases in the volume of polymer, the permittivity, perme-ability, and dielectric and magnetic loss of all the composites decreased. Thepermittivity and permeability of all the composites have shown good frequencystability and low dielectric and magnetic losses within the measurement range.

HEBM in Carbon/Graphite Matrix Composites (CGMC)

Polymer composites, ordinarily, consist of additives and polymer matrices, whichinclude thermoplastics, thermosets, and elastomers, and are considered an importantgroup of relatively inexpensive materials for many engineering applications. Two ormore materials were combined to produce composites that possessed properties thatwere unique. For example, high modulus carbon fibers or silica particles were addedinto a polymer to produce reinforced polymer composites that exhibited significantlyenhanced mechanical properties including strength, modulus, and fracture tough-ness. However, there were some bottlenecks in optimizing the properties of polymercomposites by employing traditional micron-scale fillers. The conventional fillercontent in polymer composites was generally in the range of 10–70 wt%, which inturn resulted in a composite with a high density and high material cost. In addition,the modulus and strength of composites were often traded for high fracture tough-ness (Ajayan et al. 2006; Schadler and Braun 2002).

To produce a good polymer/CNT nanocomposite, one in which a significantenhancement of the properties of the matrix was achieved, it was necessary tobreak the CNT aggregates at least into isolated bundles or strands. However, theideal nanocomposite would have individual CNTs uniformly distributed throughoutthe matrix. A good dispersion and distribution would result in a more efficient stresstransfer and uniformed stress distribution, avoiding stress concentration (Terife andNarh 2011). In addition, CNT/polymer nanocomposites were one of the most studiedsystems because of the fact that polymer matrix could be easily fabricated withoutdamaging CNTs based on conventional manufacturing techniques, a potentialadvantage of reduced cost for mass production of nanocomposites in the future.Following the first report on the preparation of CNT/polymer nanocomposites in1994 (Ajayan et al. 1994), many research efforts had been undertaken in order tounderstand their structure-property relationships and to identify their useful appli-cations in different fields. In the beginning of the twenty-first century, those effortshave become more pronounced after the realization of CNT fabrication on industrialscale with low costs. Depending on the specific application, CNT/polymer nano-composites can be classified as structural or functional composites (Du et al. 2007).


CNTs that were treated by HEBM are processed for different milling times. Thebroken nanotubes and many of carbon onion-like particles were obtained in thesample milled for 15 min. When the milling time was upped to 60 min, carbonnanotubes turned into amorphous carbon (Li et al. 1999). Ball milling has beensuccessfully applied to carbon materials for a variety of purposes, viz., to transformCNTs into nanoparticles, to generate highly curved or closed shell carbon nano-structures from graphite (Gao et al. 2000), to enhance the saturation of lithiumcomposition in SWCNTs (Huang et al. 1999), to modify the morphologies of cup-stacked CNTs (Kim et al. 2002), and to generate different carbon nanoparticles fromgraphitic carbon for hydrogen storage applications (Awasthi et al. 2002). Ballmilling of CNTs in the presence of chemicals not only enhances their dispersibilitybut also introduces some functional groups onto the CNT surface. A simple chemo-mechanical method was achieved in in situ amino functionalization of CNTs usingball milling (Ma et al. 2008, 2009). The results showed that CNTs milled withammonium bicarbonate (NH4HCO3) were more effectively disentangled and short-ened than those without the chemical and the CNT length was controlled bychoosing an appropriate milling time.

CNTs were held together in bundles or entanglements consisting between 50 anda few hundred individual CNTs by van der Waals force of CNT bundles depict suchentanglements. The influence of ball milling on the properties of nanotubes and theircomposites with PC was studied by (Ma et al 2010; Thess et al. 1996). For nanotubematerial before and after milling for 5 and 10 h, the length distributions werequantified by using TEM analysis, which showed decreases in the mean lengthsby ~54% and ~35%, respectively. With increased ball-milling time, in addition to adecrease of agglomerate size, an increase of the packing density took place, whichresulted in a worse dispersibility in aqueous surfactant solutions. HEBM could beemployed as an innovative process to incorporate CNTs into a polyethylene (PE)matrix, hence, avoiding high temperatures, solvents, ultra-sonication, and chemicalmodification of carbon nanotubes. HEBM of powders constituting PE and multiwallcarbon nanotubes (MWNTs) has been proved to be an alternative and efficienttechnique to produce novel composites without using high temperatures, solvents,and any physical and/or chemical treatment of the components. The improvement ofthermal, mechanical, and electrical properties of composites was very relevant forlow nanotube content (usually between 2%wt and 3%wt) (Gorrasi et al. 2007). Theauthor further reported LLDPE/MWCNT nanocomposites by centrifugal ball mill-ing in solid state at room temperature. They observed a 20% increase in elasticmodulus following the incorporation of 1 and 2 wt% MWCNTs. MWCNT wasincorporated into LLDPE matrix through HEBM technique at room temperature,without any chemical modification or physical treatment of the nanotubes. It wasalso reported by the author that a cryogenic ball-milling process to produce LLDPE/CNT nanocomposites was investigated. The cryogenic ball-milling process allowedthe production of LLDPE/MWCNT nanocomposites with enhanced elastic modulus.The elastic modulus of the nanocomposites increased by up to 28%, relative to theunfilled polymer, although there was lack of correlation between the elastic modulusincrease and the mixing parameters (Terife and Narh 2011). An in-depth


investigation of the thermal behavior of nanocomposites of LLDPE and CNT,prepared by the method HEBM, has been done. Moreover, the CNT acted asnucleating agent for the LLDPE crystallization, as revealed by the increased in thecrystallization temperatures of the nanocomposites with respect to the neat polymer.Self-nucleation behavior confirmed the strong nucleating effect of the CNT onLLDPE (Pucciariello et al. 2011). The effect of the electrical field on the conduc-tivity of LLDPE/CNT composites during the temperature cycling has also beeninvestigated. They found out that heating/cooling cycling, under electrical field,clearly improved the electrical characteristics of LLDPE/CNT composites. Thethermal and electrical behaviors of the composites were found to be stronglydependent on the applied voltage (Ferrara et al. 2007). Xiao et al. (2007) studiedthe mechanical properties of LDPE reinforced with MWCNTs. The nanocompositeswere prepared through mechanical mixing at 140 �C. They observed that the elasticmodulus increases with the nanotube concentration. The change in elastic modulus,with respect to unfilled LDPE, was ~11% and ~21% for MWCNT concentrations of1 and 3 wt%, respectively. Medium-density polyethylene (MDPE/MWCNT) nano-composites were produced by a mechanical milling method by using HEBM. Themilling process could be a suitable method for producing MDPE/MWCNT nano-composites. Addition of carbon nanotubes to MDPE caused a change in its mor-phology at constant milling parameters. The increase in both yield strength andYoung’s modulus of MDPE due to the addition of MWCNTs was much higher thanthose achieved by using conventional methods (Noroozi and Zebarjad 2010). HDPE/MWCNT composites shows good enhancement of mechanical properties withincreaseof CNT concentration and the reinforcement increases with an increaseCNT because of good load transfer effect and interface linked between CNT andpolymer. a consequence of good adhesion between the nanotubes and the matrixmaterial (Kanagaraj et al. 2007). It was further reported (Wang et al. 2005) thatultrahigh molecular weight polyethylene (UHMWPE)-CNT composite fibers wereprepared by gel spinning. In order to realize a homogeneous dispersion and goodload transfer between the CNTs and the polymer matrix, the purification andfunctionalization of CNTs were carried out. The mechanical and thermal propertiesof UHMWPE-CNT fibers, prepared by gel spinning and ultra-drawing, wereimproved when compared with that of pure UHMWPE fiber.

The effect of ball milling on the structural characteristics and on the dispersionand percolation behaviors of MWCNTs in melt-mixed composites by using maleicanhydride-modified isotactic polypropylene (iPP) as matrix was investigated.Microscopy examination revealed that ball-milled nanotubes were considerablyshorter and showed a compact primary agglomerate morphology when comparedto the As-synthesizedMWCNTs. Due to the ball-milling treatment, the differences inthe composite morphologies as well as in the electrical and rheological percolationbehaviors were assigned to the altered MWCNT structure. The dispersibility of ball-milled MWCNTs was restricted due to their more compact agglomerate morphol-ogies (Menzer et al. 2011). Different methods were used for cyclic polybutyleneterephthalate (pCBT)/MWCNT nanocomposites, which were prepared by in situpolymerization of CBT after solid-phase HEBM of the polymerization catalyst


contained CBTwith MWCNT. Based on their studies ball milling reduced the aspectratio of MWCNT was effectively, produced and this contributed to its excellentdispersion in the pCBT produced. Moreover, ball-milled MWCNT/catalyst-freeCBT compound might be used as MWCNT masterbatch for various polymers(Balogh et al. 2013). (Díez-Pascual et al. 2009) (Hsu et al. 2017) employed poly(ether ether ketone) (PEEK)/SWCNTcomposites, at different wt% SWCNT content,which have been prepared by melt blending. An efficient dispersion of the CNTs inthe matrix was achieved by the combination of polymer ball-milling and mechanicalpretreatments in ethanol, as revealed by micrographs of fractured film surfaces.Thermogravimetric analysis (TGA) showed a substantial increase in the matrixdegradation temperatures by the incorporated SWCNTs. Higher thermal stabilitywas found for samples with improved CNT dispersion. The effect of polyetherimide(PEI) as a compatibilizing agent on the morphology and thermal, electrical, anddynamic mechanical properties of PEEK/SWCNT nanocomposites has been inves-tigated for different CNT loadings. After a preprocessing step based on ball millingand premixing under mechanical treatment in ethanol, the samples were prepared bymelt extrusion. TGA demonstrated an increased in the matrix degradation temper-atures under dry air and nitrogen atmospheres with the addition of SWCNTs; thelevel of thermal stability of those nanocomposites was maintained when PEI wasincorporated (Diez-Pascual et al. 2009). Compounding methods included ball mill-ing, high-shear mixing in the melt, as well as extrusion using a twin-screw extruder.PET/CNF composite resins were then melt-spun into fibers used conventional PETfiber spinning conditions. The morphology and mechanical properties of thosecomposite fibers have been studied and showed that CNFs could be incorporatedinto PET matrix with good dispersion. But tensile strength and modulus were notincreased significantly by the addition of nanofibers (Ma et al. 2003). PET andhalloysite nanotube (HNT) composites prepared through HEBM at ambient temper-ature and with no solvents. Diffraction analysis showed an amorphous structure ofPET matrix that was retained in the composites at any HNT composition. Mechan-ical analysis showed a reinforcement of PET matrix, especially at low HNT content,with a decrease of elongation at break and at high filler content. Thermal analysisrevealed that halloysite nanotubes acted as effective nucleating agents for PET; thestronger effect was observed for HNT content 3 and 5 wt% (Gorrasi et al. 2014).

PS was compounded with graphite that possessed high thermal conductivity andlayer structures, and the PS/graphite thermal conductive nanocomposites wereprepared. The diffraction analysis indicated that the degree of layers of exfoliationof the graphite was enhanced in the order of rolling intercalation, solvent intercala-tion, and pan-milling intercalation. The microscopy analysis indicated that the chainstructure of graphite agglomerates of the composites was formed by the pan-millingintercalation method, which provided a more conductive path, resulting in the higherthermal conductivity and mechanical properties of the composites (Tu and Ye 2009).According to the author, a one-step method for the preparation of PS-functionalizedgraphene nanosheets, homogeneously dispersed in a PS matrix and formed electri-cally conductive graphene/PS nanocomposites, via in situ peeling of graphite nano-platelets into graphene nanosheets in the presence of a PS solution, was presented on


the paper. To their best of their knowledge, that was the first reported that achievedthe functionalization of un-oxidized pristine graphene sheets with a polymer via aone-step in situ ball-milling method (Wu et al. 2011). A one-pot in situ method formanufacturing polymer/graphene sheet nanocomposites was proposed via exfoliat-ing GNs in EVA-g-MAH solution using wet ball-milling process. The exfoliation ofGNs into graphene sheets improved the comprehensive performance to polymermatrix greatly. Single- and few-layer graphene sheets have been successfullyachieved using the wet ball-milling method from GNs in polymer solution. Theresults showed that a much lower percolation threshold and higher thermal stabilitywere achieved in the final graphene nanocomposites compared with those of thetraditional nanocomposites reinforced with GNs (Wu et al. 2012). According to theauthors’ work, poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) andfunctionalized graphene nanosheet (FGS) nanocomposites were successfullyobtained through the ball-milling technique, and the effect of FGS addition wasstudied. The morphological characterization revealed good dispersion of the fillerwhich was also well distributed, although for high loadings, filler concentration areaswere observed. FGS acted as a nucleating agent and increased the overall crystalli-zation rate and the crystallization degree, leading to a more heterogeneous crystal-lization. Their work provided evidence that the ball-milling technique could besuccessfully applied to develop graphene-based nanocomposites with good disper-sion and distribution of the filler into the polymer matrix (Ambrosio-Martín et al.2015).

Conclusion

In the past years, the interest in the production of polymer nanocomposites by ballmilling has considerably increased as the number of publications with related subjecthas increased. Mechanical alloying is a simple, sophisticated, and convenient pro-cessing technique that continues to attract the serious attention of researchers. MA isa complex process that involves many variables, and many of them areinterdependent. Therefore, modelling of the MA process is very difficult. Uniformdispersion can be achieved using various types of mechanical methods, includingultra-sonication, shear mixing, calendaring, ball milling, stirring, and extrusion. Ithas become a major potential process for processing advanced materials whichawaits to be used in industry. It is now time for materials scientists who are interestedin developing high-energy mechanical milling into an industrial process to learnfrom researchers who have mastered the art of low-energy mechanical milling.Selection of a proper method or a combination of several methods as well as theirprocessing conditions has to be based on the desired properties of end products.HEBM valuable equipment to study polyesters materials with different nanofillersand clays there’s least research on that field. The polymer-nanoparticle systems thathave been studied this far provided a basis for refinement, and further work willfurnish valuable insight into the mechanisms of reinforcement and new methods ofnanocomposite design.


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