austenitic stainless steel patterning by plasma assisted

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Austenitic stainless steel patterning by plasmaassisted diffusion treatmentsTo cite this article T Czerwiec et al 2009 IOP Conf Ser Mater Sci Eng 5 012012

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Austenitic stainless steel patterning by plasma assisted diffusion treatments

T Czerwiec1 G Marcos T Thiriet Y Guo T Belmonte Institut Jean Lamour (IJL) Ecole des Mines de Nancy Parc de Saurupt CS 14234 54 042 Nancy France E-mail thierryczerwiecminesinpl-nancyfr Abstract The new concept of surface texturing or surface patterning on austenitic stainless steel by plasma assisted diffusion treatment is presented in this paper It allows the creation of uniform micro or nano relief with regularly shaped asperities or depressions Plasma assisted diffusion treatments are based on the diffusion of nitrogen andor carbon in a metallic material at moderate to elevated temperatures Below 420degC a plasma assisted nitriding treatment of austenitic stainless steel produces a phase usually called expanded austenite Expanded austenite is a metastable nitrogen supersaturated solid solution with a disordered fcc structure and a distorted lattice The nitrided layer with the expanded austenite is highly enriched in nitrogen (from 10 to 35 at) and submitted to high compressive residual stresses From mechanical consideration it is shown that the only possible deformation occurs in the direction perpendicular to the surface Such an expansion of the layer from the initial surface of the substrate to the gas phase is used here for surface patterning of stainless steel parts The surface patterning is performed by using masks (TEM grid) and multi-dipolar plasmas

1 Introduction Surface patterning is an exciting challenge for the thin film and surface engineering community Surface patterning also known as surface texturation or surface structuration is a part of surface engineering that consists in the production of a patterned surface with some regular array of surface height features on the size scale of several micrometers to some nanometres [1] Patterned surfaces have many potential applications in various fields such as surface energy optics biology tribology mechanics hydrodynamicshellip [2] Surface patterning manufacturing methods are widely used in the semiconductor industry [3] However these technologies are mostly specific to silicon highly sophisticated and expensive Alternative cheap and flexible technologies are thus needed to satisfy the vast demand for emerging applications The different techniques used for surface transformation can be categorized into four main groups according to the classification proposed by Bruzzone et al [2]

bull Adding material the patterned surfaces are created by addition of material to the desired surface creating small areas of relief

bull Removing material the patterned surfaces are produced by removal of material of the surface creating small depressions

1 To whom any correspondence should be addressed

5th International EEIGMAMASEFORGEMAT Conference on Advanced Materials Research IOP PublishingIOP Conf Series Materials Science and Engineering 5 (2009) 012012 doi1010881757-899X51012012

ccopy 2009 IOP Publishing Ltd 1

bull Moving material the change in the surface structure is attributable to elastic or plastic deformation and redistribution of material from some parts of the surface to others

bull Self-forming a disordered system of components already on the surface or brought to the surface forms an organized pattern as a consequence of specific local interactions among the components themselves

The new concept of surface patterning we present in this communication belongs to the third category of this classification It is applicable to austenitic materials forming the so called ldquoexpanded austenite phaserdquo [4-5] The redistribution of material from some parts of the surface to others is based on a selective plasma assisted diffusion treatment of stainless steel substrates masked by TEM grids of different mesh sizes Plasma assisted diffusion treatments are based on the diffusion of nitrogen andor carbon in a metallic material at moderate to elevated temperatures Below 420degC a plasma assisted nitriding (PAN) treatment of austenitic stainless steel produces a peculiar phase usually called expanded austenite or γN

phase From mechanical consideration it is shown that the only possible deformation occurs in the direction perpendicular to the surface Such an expansion of the layer from the initial surface of the substrate to the gas phase is used here for surface patterning of stainless steel parts For patterning we use multi-dipolar plasmas arranged in a two-dimensional array belonging to the new generation of low-pressure high-density plasma sources providing independent substrate biasing and independent ion flux and ion energy control The resulting plasma diffuses towards the substrate-holder that can be independently heated andor biased It is thus possible to carefully control the sputtering of the sample surface

2 Background on expanded austenite Austenitic stainless steels and austenitic nickel-based alloys are used in industrial applications where corrosion resistance (especially in wet environment) and toughness are primary requirements An improvement of the surface properties (hardness wear and corrosion resistance) of these alloys is obtained by thermo-chemical diffusion treatments such as plasma assisted nitriding However it is known from the seventies that the corrosion resistance of these nitrided alloys is reduced at such elevated temperatures [4-5] This is attributed to the precipitation of chromium nitrides in the near surface region of the diffusion layer with an accompanying decrease of the chromium content in γ phase compared to the bulk composition of the alloy Consequently nitriding treatments of stainless steels and nickel based alloys have to be performed at low temperature Below 420degC a plasma assisted nitriding treatment of these alloys produces a peculiar phase usually called expanded austenite S phase m phase or γN phase Expanded austenite is a metastable nitrogen supersaturated solid solution with a disordered fcc structure and a distorted lattice that will be called γN phase in this communication This phase is hard wear resistant and a paramagnetic to ferromagnetic transition takes place for nitrogen content higher than 11-14 at [6] Other peculiar features of the expanded austenite are high nitrogen content (from 10 to 35 at) and high compressive residual stress in the nitrided layer A noteworthy property of expanded austenite is that different lattice parameters are calculated from different diffraction lines (figure 1) The lattice parameter calculated from the (200) diffraction lines is always higher than the lattice parameters calculated from the other ones An explanation for this phenomenon involves the formation of high compressive residual stresses in the nitrided layer resulting in a highly distorted fcc structure A simple method based on a plot of the different lattice parameters obtained from X ray diffraction data as a function of the orientation factor Ahkl can be used to determine the mean internal stress in the expanded austenite (figure 2) This model allows the mean internal stress ltσgt and the mean compositional strain ltεcgt to be deduced from the measured dependence of the lattice parameters on the orientation factor [5] Here we only present a simplified version of our deformation model Let us consider the part of the sample which will form the nitrided layer (figure 3a) The introduction of nitrogen into the nitrided layer will going to lead a lattice


2

expansion that would be isotropic for a layer removed from the substrate The associated deformation is known as the dilatational or compositional strain εc As the thin nitrided layer is attached to the substrate a biaxial compressive stress σ will develop to elastically deform the layer in order to compensate the effect of compositional strain The relation between the resulting compressive state of stress and strain is described by tensors through the Hookersquos law [5]

40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)

20 micromicromicromicrom

40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)

20 micromicromicromicrom20 micromicromicromicrom

Figure 1 X-ray diffraction pattern of an AISI 316L sample after a 1h nitriding treatment with the MDECR process at 400degC with 600 W in a 60 N2- 40 H2 gas mixture at 575 Pa with substrate bias of -50 V and the related optical cross-sectional micrograph The structure was revealed by the Curran reagent

000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a

a0C(a minusgt=σlt=gtεlt

( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a

aa minusgtlt=gtεltaγN (nm)

gtεlt ψhkl

ltAhklgt

000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a


( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a


gtεlt ψhkl

ltAhklgt

Figure 2 Plots of (a) expanded austenite lattice parameters aγN versus Ahkl and (b) the mean total

strain in the [hkl] direction gtεlt t]hkl[ for the sample described in fig 1


3

A transformation in the substrate reference frame is made using an appropriate grain-interaction model (Reuss grain-interaction model ie homogeneous stress distribution in a direction parallel to the surface) An equibiaxial state of stress (σij = 0 for i ne j σ11 = σ22 = σ and σ33 = 0) is assumed with a stress dependence on z the distance from the surface to the interface between the stressed layer and the substrate As X-ray diffraction measurements results from an averaging over diffracting crystallites on the penetration depth mean values are used for stress lattice parameters and strains Finally for quasi-isotropic specimens and X-ray measurements made in θminus2θ configuration (ψ = 0) the mean

elastic diffraction strain gtεlt ψhkl is given by (1) where hkl012

hkl1 ASSS += are the X-ray elastic

constants S0 = S11 - S12 ndash S442 S11 S12 and S44 are the mechanical constants gtεlt t]hkl[ is the mean

total strain in the [hkl] direction measured by X-ray diffraction through

( 00hklt

]hkl[ a)aa( minusgtlt=gtεlt ) where gtlt hkla is the mean lattice parameter and a0 the lattice

parameter from the substrate

Fcc austenitic lattice

Elasticstrain

(εεεεe)

Nitrogen introduction

Substrate

Nitrided layer (without stress and nitrogen)

Substrate

σσσσ

Internal stress necessary to return film

to substrate dimension

Nitrided layer (with nitrogen)virtually removed from the substrate

Dilatationalor

compositionalstrain

(εεεεc)

Substrate action on the layer


Internalstress (σσσσ)

(a)

(b) ∆∆∆∆xe


Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe

Figure 3 Schematic illustration of the different strains and stress present in a nitrided austenitic layer (a) compositional or dilatational strain due to nitrogen introduction in the nitrided layer (b) elastic strain due to the internal compressive stress resulting from nitrogen introduction in the nitrided layer The dashed line shows the initial position of substrate surface

gtεltminusgtεlt=gtσlt=gtεlt ψct

]hkl[hkl1

hkl S2 (1)

From the plot of the mean lattice parameter ltahklgt as function of the orientation factor Ahkl a linear relation (2) is generally obtained (fig 2b) The use of equation (1) allows the determination of ltσgt and ltεcgt by considering that ltσgt lt 0 and using the following values for the elastic constant of AISI


4

316L S11 = 107 10-12 Pa-1 S12 = - 425 10-12 Pa-1 and S44 = 86 10-12 Pa-1 [7-8] Mean values of - 247 GPa and 0056 are obtained for the internal stress and the compositional strain in the nitrided layer of the 316L sample presented in fig1

[ ] gtεlt+gtε=ltσ+ε+σ=β+α=ε ψchkl

hkl0c

12hklt

]hkl[ AS2S2A (2)

From mechanical considerations on thin films it appears that the only possible deformation occurs in the direction perpendicular to the surface [9] This deformation ∆x is shown in figure 3b Such an expansion of the layer from the initial surface of the substrate to the outer is used here for surface patterning of stainless steel parts

3 Experimental set-up AISI 316L Stainless steel (13wtNi 17wt Cr 67wtFe 2wt Mo 05wt Si 02wt Mn 002wtC) samples were cut from a cylindrical rod and machined to 20 mm in diameter 4 mm in thickness disks then mechanically polished to a mirror-like finish (diamond 3 microm) The samples were cleaned in methanol for 15 min by using ultrasonic cleaning just before being placed into the reactor chamber The multi-dipolar plasmas we used for PAN is based on the DECR (distributed electron cyclotron resonance) concept [10] The microwave (245 GHz) power is supplied through eight microwave antenna rods arranged in two-dimensional network (square) The resonant magnetic field is produced by eight permanent magnets located in front of the microwave antennas The resulting plasma diffuses towards the substrate-holder that can be independently heated andor biased With this multi-dipolar electron cyclotron resonance (MDECR) apparatus it is possible to preserve the initial surface state of work pieces Our method for creating patterns on austenitic stainless steel samples is illustrated schematically in figure 4 Copper TEM grids having bar width of 55-58 microm and holes size of 192-194 microm are placed on a stainless steel sample surface (figure 4a) An in-situ cleaning pre-treatment intended to remove the native oxide layer is performed before nitriding in a 75Ar ndash 25 H2 plasma under a 2 Pa pressure For this cleaning step the injected power is 600 W and the dc bias applied the substrate is ndash 100V During this step the sample is progressively heated to the nitriding temperature by external heating A nitriding treatment is then performed in a 70N2 ndash 30 H2 plasma under a 575 Pa pressure at 400degC For the nitriding step the injected power is 600 W and the dc bias applied the substrate is ndash 50V or 0V (floating potential) (figure 4b) At the end of the treatment the samples were slow cooled down under vacuum The grid is removed and a pattern can be seen on the austenitic stainless steel sample (fig4c) Optical views of the grid and of the sample surfaces after the patterning process are respectively shown in figure 4a and 4c


5

(a) (b) (c)(a) (b) (c)(a) (b) (c)(a) (b) (c)

Figure 4 Principal plan for the surface patterning of stainless steel by plasma assisted nitriding (a) positioning of the TEM grid on the sample and optical image of a part of the grid (b) treatment in a N2-H2 plasma and (c) picture of the treated sample with the grid removed

The analysis of the microstructure of the nitrided samples is performed by optical microscopy and scanning electron microscopy (SEM) and X-ray diffraction using Co Kα radiation with a θminus2θ configuration The patterned surface is imaged with a profilometer (SURFASCAN 3S) with a 2 microm diameter diamond tip 3 dimensional map of the patterned surface is obtained by the laquo Mountains Map raquo softwear

4 Austenitic stainless steel patterning The topography and measures of height of a patterned AISI 316L sample after a 1h nitriding treatment with the MDECR process at 400degC with 600 W in a 60 N2- 40 H2 gas mixture at 575 Pa and substrate bias of -50 V are presented in figure 5 Square dots with lateral dimension of 200 microm times 200 microm and height of 220 nm to 275 nm are obtained as shown in the line scan of figure 5 Optical cross-sectional and top surface views of the patterned sample are depicted in figure 6 The nitrided zones correspond to the parts of the sample exposed to the plasma (with a mean nitrided layer thickness e = 23 microm) while the not nitrided zones correspond to the parts of the sample masked by the wires of the grid This is evidenced by the optical top view of the patterned sample (figure 6b) where grain boundaries are revealed by the ion bombardment cleaning step and the nitriding treatment Nitrided and not nitrided zones corresponding respectively to the relief zones and to the zones in depression can be seen on figure 5


6

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

Valeurs moyennes sur 11 creacuteneaux

Profondeur maximale 0333 microm

Profondeur moyenne 023 microm

Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7

Profondeur maximale 0314 microm 0257 microm 0274 microm 0209 microm 0303 microm 0266 microm 0361 microm

Profondeur moyenne 0266 microm 0255 microm 0273 microm 0207 microm 0289 microm 0259 microm 0313 microm

Largeur 250 microm 278 microm 278 microm 278 microm 278 microm 278 microm 250 microm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

Figure 5 Topography and measures of height of a patterned austenitic stainless steel (AISI 316L) sample after a 1h nitriding treatment with the MDECR process at 400degC with 600 W in a 60 N2- 40 H2 gas mixture at 575 Pa with substrate bias of -50 V

50 micromicromicromicrom 50 micromicromicromicrom

(a)

(b)

50 micromicromicromicrom 50 micromicromicromicrom50 micromicromicromicrom 50 micromicromicromicrom50 micromicromicromicrom 50 micromicromicromicrom50 micromicromicromicrom

(a)

(b)

Figure 6 Optical micrographs of an austenitic stainless steel sample patterned in conditions given in figure 5 (a) cross-sectional views and (b) top surface views

Our elastic model allows the estimation of the deformation ∆x in the direction perpendicular to the

surface as function of e and gtεlt t]hkl[

t]hkl[

t]hkl[

1ex

ε+

εsdotgtlt=gt∆lt (3)

The application of relation 3 to the data from figure 3 allows the estimation of the deformation ∆x to be between 130 to 170 nanometres By taking into account the profilometer resolution (plusmn50 nm) this estimation is well correlated to the experimental data (height of 220 nm to 275 nm)

5 Conclusion Surface patterning also known as surface texturation or surface structuration allows the production of patterned surfaces with some regular array of surface height features on the size scale of several


7

micrometers to some nanometres A new concept of surface patterning on austenitic stainless steel by plasma assisted diffusion treatments was presented in this paper Below 420degC a plasma assisted nitriding treatment of austenitic stainless steel produces the so-called expanded austenite a metastable nitrogen supersaturated solid solution with a disordered fcc structure and a distorted lattice The high compressive residual stress induced by the introduction of large amounts of nitrogen (from 10 to 35 at) produces an expansion of the nitrided layer from the initial surface of the substrate to the gas phase This deformation in the direction perpendicular to the surface was estimated by a mechanical model Patterned surfaces obtained by a selective diffusion of nitrogen using TEM grid as a mask were characterized by optical microscopy and a profilometer Square dots with lateral dimension of 200 microm times 200 microm and height of 220 nm to 275 nm are obtained by this technique References [1] Evans CJ Brian BB Annals of the CIRP 48 (1999) 541 [2] Bruzzone AAG Costa HL Lonardo PM Lucca DA CIRP Annals Manufacturing

Technology 57 (2008) 750 [3] Luttge R J Phys D Appl Phys 42 (2009) 123001s [4] Czerwiec T Renevier N Michel H Surf Coat Technol 131 (2000) 267 [5] Czerwiec T He H Marcos G Thiriet T Weber S Michel H Plasma Process Polym 6

(2009) 401 [6] Basso RLO Pimentel VL Weber S Marcos G Czerwiec T Baumvol IJR Figueroa CA

J Appl Phys 105 (2009) 124914 [7] Rejevac V Hoelzel M Danilkin SA Hoser A Fuess H J Phys Condens Matter 16

(2004) 2609 [8] Teklu A Ledbetter H Kim S Boatner LA McGuire M Keppens V Mett Mat Trans A

35 (2004) 3149 [9] Johnson WC Huh JY Met Mat Trans A 34 (2003) 2819 [10] Lacoste A Lagarde T Bechu S Arnal Y Pelletier J Plasma Sources Sci Technol 11

(2002) 407


8

Austenitic stainless steel patterning by plasma assisted diffusion treatments

T Czerwiec1 G Marcos T Thiriet Y Guo T Belmonte Institut Jean Lamour (IJL) Ecole des Mines de Nancy Parc de Saurupt CS 14234 54 042 Nancy France E-mail thierryczerwiecminesinpl-nancyfr Abstract The new concept of surface texturing or surface patterning on austenitic stainless steel by plasma assisted diffusion treatment is presented in this paper It allows the creation of uniform micro or nano relief with regularly shaped asperities or depressions Plasma assisted diffusion treatments are based on the diffusion of nitrogen andor carbon in a metallic material at moderate to elevated temperatures Below 420degC a plasma assisted nitriding treatment of austenitic stainless steel produces a phase usually called expanded austenite Expanded austenite is a metastable nitrogen supersaturated solid solution with a disordered fcc structure and a distorted lattice The nitrided layer with the expanded austenite is highly enriched in nitrogen (from 10 to 35 at) and submitted to high compressive residual stresses From mechanical consideration it is shown that the only possible deformation occurs in the direction perpendicular to the surface Such an expansion of the layer from the initial surface of the substrate to the gas phase is used here for surface patterning of stainless steel parts The surface patterning is performed by using masks (TEM grid) and multi-dipolar plasmas

1 Introduction Surface patterning is an exciting challenge for the thin film and surface engineering community Surface patterning also known as surface texturation or surface structuration is a part of surface engineering that consists in the production of a patterned surface with some regular array of surface height features on the size scale of several micrometers to some nanometres [1] Patterned surfaces have many potential applications in various fields such as surface energy optics biology tribology mechanics hydrodynamicshellip [2] Surface patterning manufacturing methods are widely used in the semiconductor industry [3] However these technologies are mostly specific to silicon highly sophisticated and expensive Alternative cheap and flexible technologies are thus needed to satisfy the vast demand for emerging applications The different techniques used for surface transformation can be categorized into four main groups according to the classification proposed by Bruzzone et al [2]

bull Adding material the patterned surfaces are created by addition of material to the desired surface creating small areas of relief

bull Removing material the patterned surfaces are produced by removal of material of the surface creating small depressions

1 To whom any correspondence should be addressed


ccopy 2009 IOP Publishing Ltd 1







2


40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)


40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)



000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a


( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a


gtεlt ψhkl

ltAhklgt

000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a


( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a


gtεlt ψhkl

ltAhklgt




3






( 00hklt




Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe


Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe



]hkl[hkl1

hkl S2 (1)



4



hkl0c

12hklt

]hkl[ AS2S2A (2)




5

(a) (b) (c)(a) (b) (c)(a) (b) (c)(a) (b) (c)





6

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm



(a)

(b)


(a)

(b)




t]hkl[

t]hkl[

1ex

ε+





7







(2002) 407


8







2


40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)


40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)



000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a


( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a


gtεlt ψhkl

ltAhklgt

000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a


( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a


gtεlt ψhkl

ltAhklgt




3






( 00hklt




Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe


Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe



]hkl[hkl1

hkl S2 (1)



4



hkl0c

12hklt

]hkl[ AS2S2A (2)




5

(a) (b) (c)(a) (b) (c)(a) (b) (c)(a) (b) (c)





6

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm



(a)

(b)


(a)

(b)




t]hkl[

t]hkl[

1ex

ε+





7







(2002) 407


8


40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)


40 60 80 100 120 140

0

5000

10000

15000

20000

25000

Inte

nsity

(a

u)

2θ

γ (220)

γN (111)

γ (111)

γN (200)

γ (200)

γ (311)

γ (222)



000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a


( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a


gtεlt ψhkl

ltAhklgt

000 005 010 015 020 025 030 035000

001

002

003

004

005

006

007

008

009

010

000 005 010 015 020 025 030 0350355

0360

0365

0370

0375

0380

0385

0390

0395

0400

a0 = aγ

0

0Nc

a


( )2222

222222

hkllkh

lklhkhA

++++= ( )2222

222222

hkllkh

lklhkhA

++++=

gtlt t]hkl[ε

(a) (b)

γN (200)

γN (111)

γN (200)

γN (111)

0

0hkl

t]hkl[ a


gtεlt ψhkl

ltAhklgt




3






( 00hklt




Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe


Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe



]hkl[hkl1

hkl S2 (1)



4



hkl0c

12hklt

]hkl[ AS2S2A (2)




5

(a) (b) (c)(a) (b) (c)(a) (b) (c)(a) (b) (c)





6

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm



(a)

(b)


(a)

(b)




t]hkl[

t]hkl[

1ex

ε+





7







(2002) 407


8






( 00hklt




Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe


Elasticstrain

(εεεεe)


Substrate


Substrate

σσσσ




Dilatationalor

compositionalstrain

(εεεεc)




(a)

(b) ∆∆∆∆xe



]hkl[hkl1

hkl S2 (1)



4



hkl0c

12hklt

]hkl[ AS2S2A (2)




5

(a) (b) (c)(a) (b) (c)(a) (b) (c)(a) (b) (c)





6

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm



(a)

(b)


(a)

(b)




t]hkl[

t]hkl[

1ex

ε+





7







(2002) 407


8



hkl0c

12hklt

]hkl[ AS2S2A (2)




5

(a) (b) (c)(a) (b) (c)(a) (b) (c)(a) (b) (c)





6

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm



(a)

(b)


(a)

(b)




t]hkl[

t]hkl[

1ex

ε+





7







(2002) 407


8

(a) (b) (c)(a) (b) (c)(a) (b) (c)(a) (b) (c)





6

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm



(a)

(b)


(a)

(b)




t]hkl[

t]hkl[

1ex

ε+





7







(2002) 407


8

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm




Largeur 49 microm

microm

0

02

04

06

08

1

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 microm

1 2 3 4 5 6 7




microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm

microm

0

005

01

015

02

025

03

035

04

045

05

055

06

3 mm

3 mm



(a)

(b)


(a)

(b)




t]hkl[

t]hkl[

1ex

ε+





7







(2002) 407


8







(2002) 407


8

austenitic stainless steel patterning by plasma assisted

Documents