Nanoscale PVD Multilayer Coatings

Nanoscale PVD Multilayer Coatings

Today the classical multilayer coating concept is wellestablished and widely used for the design of pro-tective coatings for wear and tribological appli-cations. It offers the possibility to adapt constitution,properties, and behavior to specific requirements,e.g., by material selection and combination, varyingof bilayer period, interface volume, interface consti-tution, crystallite size, texture, or surface energy. Inthe past decade, the new class of nanoscale coatingsoffered the material scientists an even more powerfultoolbox for the engineering thin film design through acombination of the multilayer concept with newnanoscale coatings, which provide an extremely finestructural ordering at the nanoscale, leading to sig-nificantly enhanced properties and functionalities.Nanoscale coatings are thin films with at least onedimension on the nanometer scale (o100 nm). Someexamples are low-friction carbon-based nanocompo-sites in advanced multilayer structures or the stabil-ization of a specific coating in another structure in ananolaminated multilayer composite.

Modern plasma-assisted physical vapor deposition(PVD) techniques, such as pulsed or high-power im-pulse magnetron sputtering, cathodic arc evapor-ation, pulsed laser deposition, and electron beamevaporation or hybrid deposition processes com-bining these techniques, offer specific conditions forthe individual design of advanced coatings, especiallywith regard to mechanical engineering. The resultingmicrostructures and property profiles of nanoscalePVD multilayer coatings are dependent on manyparameters such as choice of materials, individuallayer thickness, deposition process parameters (e.g.,pressure, bias voltage, substrate temperature), andkinetics of deposition and growth process. Designprinciples include a functional aspect achieved bycombining layer materials with different physical,chemical, mechanical, and tribological functions anda structural aspect by adjusting grain size; structure,amount, and constitution of layers and interfaces;and the thickness of the individual layers. The mainaspects in tailoring multilayer coating properties andperformance by functional and structural design areimprovements in hardness, strength, toughness, tri-bological properties, resistance to crack initiation andpropagation, adhesion, residual stress, and resistanceto oxidation and corrosion.

In the following sections, the most importanthighlights in multilayer development with thefocus on principal design concepts will be described.The integration of nanocrystalline, amorphous,and nanocrystalline/amorphous composite materialsin multilayers and various phenomena such as thesuperlattice effect, stabilization of materials in meta-stable nonthermal equilibrium structures, and effectsrelated to coherent and epitaxial growth will be

covered. The article is limited to multilayers com-posed of hard materials with metallic, covalent, orheteropolar bonding characteristics only and doesnot refer to multilayers with metal layers or com-posed of alternating metal and ceramic hard layers.

1. Multilayer Coatings for Wear Protection:Pioneering Work and Fundamental Knowledge

First reports on the deposition of hard or superhardmultilayer coatings and their microstructure for-mation mechanisms such as superlattice growth cameup after the mid-1980s. On the basis of results forclassical multilayer coatings, which can be describedas an alternating layer-by-layer arrangement of twosingle-phase materials with individual layer thicknessbetween some hundred nanometers and a few mi-crometers, it was soon recognized that a significantreduction of both thickness of individual layers andcrystallite sizes down to a few nanometers can resultin a drastic enhancement of the coating properties.Besides the properties of the individual layer ma-terials, the grain boundaries and interfaces play animportant role for the overall coating propertiesthrough nanoscale architecture of the coatings.

Figure 1 displays some general conclusions on thestructure–property relationships of hard PVD multi-layer coatings composed of single-layer materialswith similar bonding characteristics. It was demon-strated that for most relevant properties, optimumvalues and performance could be achieved at specificvalues of the interface area (volume). For specificmultilayer coatings, e.g., combinations of TiN, TiC,and TiB2, a range of some 100–200 layers (i.e., abilayer modulation period L between 50 and 100 nm)has been identified for a 5-mm-thick coating, whereoptimum hardness, toughness, or tribological prop-erties could be achieved.

Multilayer coatings can be classified by thedominant chemical bonding type and the micro-structural characteristics of the individual layermaterials as well as by the specific nanodesignachieved by interface modeling. With regard to thecovalent chemical bonding characteristics of mostnitrides, carbides, and borides used in multilayercoatings, strengthening and toughening mechanismsknown for brittle bulk ceramics have to be consideredwhen discussing mechanical, elastic, and plasticproperties. When a multilayer surface is exposedto a mechanical load, various effects may play toge-ther, as shown schematically in Fig. 2. A crackstarting from the coating surface may be either splitor deflected at the grain or phase boundaries within alayer (grain boundary toughening or hardening) or atthe interface zone between the layers (interfacetoughening or hardening). Moreover, local delami-nation can occur at interfaces through the opening ofnanovoids or stress-induced weak links, which can

1

Layer 2

Layer 2Crack

• Crack splitting, deflection, and reduction of crack propagation at grain boundaries (grain boundary toughening/hardening)

(in-layer, interface, phase/grain boundaries, andthrough-coating effects)

Energy dissipation in ceramic multilayer coatings

Crack

• Crack splitting, deflection, and reduction of crack propagation at interfaces (Interface toughening/hardening)

Interfaces

Interfaces

• Local delamination at interfaces by opening nanovoids (crack energy dissipation, local stress relaxation, plasticity at nanoscale)

Substrate

Crack

Crack

Layer 1

Layer 1

Figure 2Toughening and strengthening mechanisms in ceramic multilayer coatings (schematically). Reproduced withpermission from Holleck H, Schier V 1995 Multilayer PVD coatings for wear protection. Surf. Coat. Technol. 76–77,328–36. Copyright Elsevier.

Residual stresses

Opt. tribologicalbehavior

Hot hardness

Optimized protectivecoatings

Toughness

• Layer boundaries (number of single layers)• Grain boundaries• Subgrain boundaries

Interface area (volume)

Opt

. trib

olog

ical

beh

avio

r

Toug

hnes

s

Har

dnes

s

Hot

har

dnes

s

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idua

l str

esse

s

Hardness

Figure 1Change in properties of nanoscale multilayer coatings as a function of the interface area (volume) (schematically,disregarding superlattice structures). Redesigned from an original work of Holleck H 1999 Design of nanostructuredthin films for tribological applications. In: Kumar A, Chung Y-W, Moore J J, Smugeresky J E (eds.) SurfaceEngineering: Science and Technology I. The Minerals, Metals & Materials Society, Warrendale, Pennsylvania,pp. 207–18.


2

har

dnes

s (k

g m

m−2

)

6000

5000

4000

3000

Microindentation hardnessSingle-crystal TiN/VN(100)Superlattices, LTN = LVN


result in local stress relaxation and even plasticity atthe nanoscale. Furthermore, there should be aninteraction of cracks with periodic strain–stress fieldsacross the interfaces in nanoscale multilayers, andalso an interaction of through-going cracks with thesubstrate material. The modeling and understandingof the elastic and plastic properties are, however,more complex as many coatings also display largeamounts of metal bonds. Hence, dislocation motionand interaction of dislocations with microstructuralfeatures such as grain boundaries, interfaces, andcolumn boundaries as well as stress-induced bondrelease and various defects and coherency strainsbetween the individual layers should be consideredtoo.

Further progress in multilayer coatings wasstimulated by the first successful epitaxial stabiliza-tion of a layer material in a different microstructurefor the TiN/AlN system (see Sect. 3) and both theincreasing knowledge on existing PVD methods andthe emerging of new deposition technologies. Untiltoday, a large variety of highly sophisticated nanos-cale multilayer coatings with promising propertieshave been developed, covering many combinations ofnitrides, carbides, carbonitrides, oxides, and otherhard phases such as titanium diboride or diamond-like carbon. However, only a few coatings have beenintroduced already into the market. In fact, there is acontrast between very tricky multilayer growth pro-cesses available in the laboratories and the demandfor easy-to-scale-up deposition processes for indus-trial use.

Multilayer design by epitaxial stabilization andsuperlattice structure formation was a major driver incoating development and is therefore used as a maincharacteristic to classify the coatings. Section 2 de-scribes multilayer coatings without epitaxial stabil-ization effects, whereas in Sect. 3 multilayer coatingsusing such effects are presented.

Vic

er

2000

100020 30 40100

VN

TIN

Superlattice period, λ (nm)

Figure 3Microindentation hardness of TiN/VN superlattice

2. Nanoscale Multilayer Coatings withoutEpitaxial Stabilization Effects

A significant part of hard PVD multilayer coatingscombines transition metal nitrides, carbides, andcarbonitrides (especially those of the elements of thegroups IVB, VB, and VIB of the periodic system). Independence of the nucleation and growth conditions,all these coatings grow with a single-crystalline,polycrystalline, columnar, or nanocolumnar structureaccording to the Thornton model.

structure as a function of the superlattice period.Reprinted with permission from Helmersson U,Todorova S, Barnett S A, Sundgren J E, Markert L C,Greene J E 1987 Growth of single-crystal TiN/VNsuperlattices with extremely high mechanical hardness.J. Appl. Phys. 62, 481–4. Copyright (1987), AmericanInstitute of Physics.

2.1 Single-Crystalline Superlattice Coatings

The periodic arrangement of two nitride or carbidehard materials with face-centered cubic (fcc) structureand metallic bonding character (i.e., TiN, VN, ZrN,CrN, NbN, TiC, VC) in a nanoscale multilayer

structure can result in a perfect compositionallymodulated structure. A breakthrough was achievedin 1987 when an enormous increase of the hardness ofsingle-crystalline TiN/VN multilayers epitaxiallygrown at 750 1C on MgO substrates by reactivemagnetron sputtering at a bilayer modulation periodL of 5.2 nm was demonstrated (see Fig. 3). Maximumhardness values of 5560 HV0.008 were determined,whereas the hardness values for TiN and VN filmswere 2200 and 1620 HV0.008. This effect since thenwas referred to as superlattice effect in the hardcoatings community, and the corresponding structureas superlattice structure. Superlattice structures withsuperlattice effect (significant hardness enhancement)were observed for various single-crystalline nitridemultilayer coatings on MgO substrates as well: TiN/V0.6Nb0.4N or TiN/NbN.

2.2 Polycrystalline Superlattice Coatings with andwithout Superlattice Effect

Using different substrate materials (i.e., polycrystallineones) or applying less severe deposition and growth

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conditions (such as significantly lower substrate tem-peratures or increased substrate bias) results in thegrowth of polycrystalline multilayer structures thatquite often show a hardness increase at bilayermodulation periods in the range of 2–10 nm. Thesecoatings are therefore also referred to as superlatticesin the literature. Significant hardness increase is re-ported for various combinations of isostructural ni-tride layers. In 1992, a superlattice effect in reactivemagnetron-sputtered TiN/NbN coatings grown onsteel substrates at substrate temperatures less than500 1C was reported for the first time, which was at-tributed to the alternating stress field resulting fromthe lattice mismatch between fcc TiN and fcc NbN.Superlattice effects have also been shown in TiN/CrN,TiN/TaN, and other TaN-, NbN-, or MoN-basedcoatings, as well as in the combinations TiC/VC andTiC/NbC.

Further approaches address the use of ternarymetastable layer materials from the (Ti,Al)N and(Cr,Al)N families and quaternary (or even multi-elemental) multilayer and superlattice structures.Superlattice structures with more or less pronouncedhardness modification were reported for combin-ations of TiAlN with ZrN, CrN, VN, or TiAlCrN,for CrAlYN/CrN, TiCN/ZrCN, and TiHfN/CrN.Moreover, this effect was found for combinations ofcrystalline carbide and nitride hard materials, e.g., inWC/TiN or WC/CrAlN, and for combinations ofcrystalline nitride or carbide with boride materials,e.g., in TiC/TiB2, ZrC/ZrB2, and ZrAlN/ZrB2.

Hardness enhancement in crystalline superlatticestructures can be explained by the blocking of dis-location motion at the layer interfaces due to differ-ences in the shear moduli of the individual layermaterials and by coherency strain causing periodicalstress–strain fields in the case of lattice-mismatchedmultilayer films. The high interface density contrib-utes to impeding dislocation motion and dislocationglide across the layer interfaces, which would requirea critical yield stress being related to the difference inthe elastic shear moduli of the individual layer ma-terials. Moreover, the overall columnar growthstructure resulting from most PVD processes, thespecific kinetic conditions for thin film nucleation andgrowth, nano- and microscale growth defects, as wellas defects in the coating microstructure, the overallstress state of the coating, the stress profile andinteraction of the individual layers, dislocations, andmicrocracks should be taken into account.

A variety of hard nanoscale multilayer coatingscan be grown with a superlattice structure (as indi-cated, for example, by the corresponding low-angleXRD reflections), but no superlattice effect with re-gard to a significant variation in hardness is observed.Such behavior was reported, for example, on tech-nologically relevant CrN/NbN and TiAlN/VNsuperlattice coatings or TiN/ZrN, TiN/AlTiN, CrN/AlTiN, TiC/NbC, and TiC/VC systems.

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2.3 Superlattice Coatings with Amorphous Layers

An emerging new approach to hard superlatticecoatings is the integration of an amorphous layermaterial, which can lead to the periodical interruptionor even complete suppression of the columnar growthin PVD coatings. The columnar grain boundariesoften act as sites for crack initiation resulting incoating failure. Therefore, a few nanometers thinamorphous layers of boron carbide were introduced inTiC/TiN multilayer coatings, thereby improving theproperties and performance significantly by forcingthe crystalline layers to periodically renucleate on theamorphous interface layer. The research on the com-bination of nanocrystalline and amorphous multilayercoatings is intensively stimulated by the work onsuperhard nanocomposite structures in the Ti–Si–Nand other systems. For example, a remarkable hard-ness enhancement and a residual stress reduction for athickness of 0.5 nm of the a-SiNx layer (with fixed2 nm TiN layer thickness) were reported for the inte-gration of amorphous SiNx layers in TiN/a-SiNx

superlattice structures. Similar effects were found forTiAlN/a-Si3N4 multilayers. Another possibility is theincorporation of amorphous carbon (a-C) and car-bonitride layers. Moreover, multiphase nanocompo-site materials composed of nanocrystalline andamorphous phases that can be integrated into multi-layer systems are an emerging issue. For example,carbon-based (Ti,Al)(N,C)/a-C nanocomposite thinfilms consisting of nanocrystalline fcc titanium alu-minum carbonitride and a-C phases in the same layerstructure can be combined with TiN layers, resultingin very interesting material properties. Coatings withvarious bilayer modulation periods, with modifiedratio of the thickness of TiN and (Ti,Al)(N,C)/a-Clayer, and optimized carbon concentration showed anexcellent performance in wear studies and cutting testson ramp copy milling of hardened A2 steel, compar-able to that of conventional (Ti,Al)N-based bench-mark coatings. This indicates the potential to optimizeboth hardness and toughness by completely coveringnanocrystals with an amorphous phase due to anelastic coupling between hard nanocrystals via sp2- orsp3-hybridizied carbon atoms.

3. Nanoscale Multilayer Coatings with EpitaxialStabilization Effects

Nanoscale multilayers composed of materials havingdifferent crystal lattice structures quite often tend toform coherent interfaces through epitaxial stabiliza-tion of one material in the lattice structure of theother one. This means, driven by the minimization ofthe interfacial energy, the thermodynamically un-favorable state of incoherent interfaces is balanced bythe growth of a metastable structure for one of thelayer materials that is able to build a coherent


interface with the other layer. Such metastablestructures are usually observed in extremely fine-scalesuperlattice structures at very low layer thickness andhave been reported for various nitride, carbide, andmixed nitride/carbide multilayer systems.

The most prominent example is the TiN/AlNsystem. AlN under thermodynamic equilibrium con-ditions forms a Wurtzite-type structure (hexagonal),whereas TiN forms an NaCl-type structure (cubic).Since the first reports on the formation of ametastable AlN NaCl-type structure in TiN/AlNsuperlattices for modulation periods L less than 3 nmby arc ion plating (see Fig. 4) and magnetron sput-tering one decade ago, large efforts to understand thestabilization effect and to optimize the superlatticearchitecture and properties have been made. Thecoatings showed a strong superlattice effect, i.e., asignificant increase of the hardness with decreasingmodulation period. AlN has also been stabilized inthe cubic NaCl-type structure in other multilayersystems like AlN/VN, AlN/NbN, and CrN/AlN.Epitaxial stabilization, sometimes accompanied bysuperlattice effects, was observed in a variety of othernitride multilayer systems, for example, in TiN/TaN,TiN/MoN, NbN/TaN systems, or in combinationswith SiNx and CNx.

In contrast to the intensive work carried out onepitaxial growth and superlattice effects in nitridemultilayer systems, only poor information is

(a) X500,000 50

Figure 4Epitaxial stabilization of fcc AlN in TiN/AlN multilayer coimages from a TiN/AlN multilayer with a bilayer period ofgrowth direction in the picture in (a) is from bottom to topReproduced with permission from Setoyama M, Nakayamaof cubic AlN in TiN/AlN superlattice. Surf. Coat. Technol.

available on similar growth effects in carbide or othernon-nitride multilayer material combinations. How-ever, recent developments address the stabilization-induced crystalline growth of such materials. Themost prominent examples are SiC and Al2O3 thatunder conventional deposition conditions in mag-netron sputtering and other relevant PVD methodsgrow in an amorphous structure. The epitaxial sta-bilization of SiC in a cubic NaCl-type structure is stilla challenging question. TiC/SiC multilayers withdifferent microstructures were deposited by reactivemagnetron sputtering from Ti and Si targets. Forbilayer modulation periods less than 23 nm and morethan 4 nm, a Ti-containing solid solution (Si1�yTiy)Cin a nanocrystalline fcc structure grew due to inter-mixing effects. The TiC template layer changed to anSi-containing solid solution of (Ti1�xSix)C in the fccTiC structure. Consequently, this was an epitaxiallystabilized structure of an SiC-type layer on a TiC-type layer. For bilayer modulation periods less than4 nm, a complete intermixing of both these layers wasobserved, and the coating microstructure again wascharacterized to be a nanocrystalline metastable solidsolution of (Ti1�xSix)C. Recently, a true epitaxialstabilization of SiC in a cubic NaCl-type structure inTiN/SiC superlattice coatings was demonstrated. Forthese coatings, a remarkable superlattice hardeningeffect with maximum values of the hardness in therange of 60 GPa was observed (see Fig. 5).

(b) X4,00,000

nm

50 nm

atings. Bright-field (a) and high-resolution (b) TEM30 nm. Dark layers are TiN, light layers are AlN. The, whereas in the picture in (b) is from left to right.A, Tanaka M, Kitagawa N, Nomura T 1996 Formation86–87, 225–30. Copyright Elsevier.

5

60

50

40

30

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0.5 1.0 1.5 2.0 2.5

SiC

SiC

HV

(G

Pa)

HV

3 nm

TiN

TiN

SiC

SiC

Modulus

Thickness of SiC layer (nm)

TiNTiN

280

320E

(G

Pa)

360

400

440

480

Figure 5Epitaxial stabilization of SiC in cubic structure and superhardness effect in magnetron-sputtered TiN/SiC superlatticecoatings. Reprinted with permission from Lao J, Shao N, Mei F, Li G, Gu M (2005) Mutual promotion effect ofcrystal growth in TiN/SiC nanomultilayers. Appl. Phys. Lett. 86, 011902-1–011902-3. Copyright (2005) AmericanInstitute of Physics.


Similar structure stabilization including a super-lattice hardening effect was demonstrated for TiN/SiO2 and TiN/SiNx multilayer coatings. For com-pleteness, it should be mentioned that the formationof hard oxide Y2O3/ZrO2 superlattice coatings hasbeen reported already one decade ago, a subject that

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may find more attention in future due to significantprogress in PVD technology.

In some material systems, the stabilization of atextured orientation instead of a crystal structure canoccur (i.e., the new layer material would grow in atexture of the template material or in another texture


of its own structure in order to minimize the inter-facial energy). Texture stabilization was observed, forexample, in nanoscale TiC/TiB2 multilayers, whereTiC layers grew in a (111) texture on the (001)-ori-ented TiB2 layers.

4. Concluding Remarks

It was shown that an extremely fine-scale structuralordering at the nanoscale is a prerequisite for theengineering design of new multifunctional hard andtough coatings. These nanoscale design principlesinclude the formation of superlattice structures, epi-taxial growth, and stabilization effects, age hard-ening, recovery and recrystallization processes, aswell as interfacial engineering or residual stressmanagement. Considering the variety of experimentalresults on hard multilayer coatings, a systematic ap-proach toward the understanding of the role of spe-cial materials, growth conditions, microstructure, andresulting properties is required. Although a gooddatabase exists for nitride multilayer systems, onlyselective information is found for other materialcombinations. This database should not only addressparameters being relevant for the nucleation andgrowth (i.e., plasma conditions, kinetics of the de-position process), but should also refer to thermo-dynamic aspects (i.e., phase relations, energetic statesof interfaces, grain and phase boundaries).

The elastic and plastic properties of multilayercoatings today are critically discussed with respect tovarious effects promoting or impeding dislocationmotion. It is generally accepted that a nanoscalegrain growth and coherent layer interfaces (as well asa reduction of a columnar morphology on themicroscale) can result in a significant hardness en-hancement. Taking into account the fact that manyhard materials have strong covalent bonds, aspectsrelated to the deformation of ceramic materials (i.e.,crack initiation, crack propagation, reduction ofcrack energies) and mechanisms of toughening ofceramics are more and more considered in theore-tical modeling. The identification and modeling ofstress states and stress distribution profiles and theirimpact on the micro- and macroscopic properties areof great importance. Thus, models like the periodicstress field distribution for nanoscale TiN/CrNmultilayer coatings or the triaxial stress field fortextured TiN films should be derived, verified, andrefined. These objectives demand substantial pro-gress on advanced characterization methods mostlycombined with complex evaluation and interpret-ation. Such methods include advanced transmissionelectron microscopy (TEM), X-ray diffraction(XRD) (i.e., the sin2c method), and further high-resolution X-ray scattering methods. In order tocharacterize mechanical properties on the nano-scale the nanoindentation method needs further

improvements both concerning theory and experi-mental procedure. For example recently, the small-angle-cross-section (SACS) method was proposed,which offers a new tool for a high-resolution depthprofiling of the mechanical properties on thenanoscale in order to obtain information especiallyon the interface regions.

Material concepts for the development of multi-layer coatings with advanced multifunctional prop-erties address the integration of new nanocrystalline,metastable, amorphous, or nanocomposite layers. Anexample is the so-called chameleon coatings, whichavoid coating failure by adaptive tribological prop-erties based on self-regulating surface chemistry andmicrostructure. Superimposing nanoscale gradientsin the chemical composition, growth of the coatingswith gradients in the substrate temperature, orinterfacial engineering by modulation of the substratebias-induced intermixing or stress relaxation at layerinterfaces may result as well in an enhancement of thephysical properties. Further interesting approachesare, e.g., phase transformation-reinforced multilayersystems (i.e., obtaining beneficial effects on themechanical properties by applying high-temperatureor stress-activated reversible phase transformationsin one layer) and the design of smart nanolaminatedcomposite systems, i.e., by incorporating functionallayers such as ferromagnetic Fe–Co films, whichcould be used as contactless wear sensors. Moreover,the integration of the Mnþ 1AXn phases (‘‘MAXphases,’’ where n¼ 1, 2, or 3) into multilayer struc-tures will be of interest. MAX phases are a class ofhexagonal-structure ternary carbides and nitrides(‘‘X’’) of a transition metal (‘‘M’’) and an A-groupelement with an inherently nanolaminated crystalstructure, i.e., with Mnþ 1Xn slabs intercalated withpure A-element layers. The most well known areTi2AlC, Ti3SiC2, and Ti4AlN3.

See also: Advanced Coatings for Structural Materi-als; Plasma Spray Coatings; Surface Coatings forHigh-temperature Alloys; Surfaces, Laser Coating of

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Nanoscale PVD Multilayer Coatings

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