Optjmizatjon of magnetron sputuer-depositjon process of thin fjlm - - PowerPoint PPT Presentation

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Optjmizatjon of magnetron sputuer-depositjon process of thin fjlm - - PowerPoint PPT Presentation

Optjmizatjon of magnetron sputuer-depositjon process of thin fjlm coatjngs on a moving cylindrical substrate PhD. Student Seminar 07/04/2016 Thomas LE COZ Supervisors : A. Lacoste M. Mantel A. Bes C. Vachey Outline Context Why do we


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Optjmizatjon of magnetron sputuer-depositjon process of thin fjlm coatjngs on a moving cylindrical substrate

  • PhD. Student Seminar 07/04/2016

Supervisors :

  • A. Lacoste
  • M. Mantel
  • A. Bes
  • C. Vachey

Thomas LE COZ

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SLIDE 2

Outline

Context

→ Why do we want to coat wire ? → Scientjfjc issues

Employed technology

→ Main specifjcatjons of reactjve sputuering in an inverted cylindrical magnetron (ICM)

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  • PhD. Seminar - LE COZ T.

07/04/2016

Commercial magnetron

→ Characterizatjon of the fjrst used commercial magnetron

Ugitech made magnetron

→ Characterizatjon of the magnetron designed by the company

Conclusions and Forthcoming work

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SLIDE 3

Context

Wide amount of stainless steel wire used in many fjelds : → Architecture → Urbanizatjon → Art → Cold heading → Automotjve …

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  • PhD. Seminar - LE COZ T.

07/04/2016

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Context

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Scientjfjc issues

Sizing the system for : → Fast roll-to-roll process → Uniform coatjngs → High quality coatjngs Consideratjons : → Geometry → Electric → Magnetjc → Thermal

  • PhD. Seminar - LE COZ T.

07/04/2016

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Employed technology

Physical Vapor Depositjon (PVD)

E Target Substrate Cathode Water cooling Substrate holder (anode) e- Ar Ar+ e- e- + Vsubstrate Vcathode Vplasma

Plasma bulk Cathode sheath Anodic sheath

Substrate Cathode V → Ionizatjon of argon atoms by surrounding electrons → Potentjal drop in the sheath accelerates the ions used to sputuer the target

  • PhD. Seminar - LE COZ T.

07/04/2016

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Employed technology

Magnetron sputuering

→ Plasma close to the target → High density (1010 – 1011 cm-3) → Low pressure (0.1 Pa) → Race tracks leading to non- homogeneous coatjngs

Inverted cylindrical confjguratjon

B

Repulsive wall Cathode / Target Anode / substrate

→ Conformal geometry → No loss of matuer on the walls

  • PhD. Seminar - LE COZ T.

07/04/2016

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Employed technology

Reactjve sputuering

Lindberg et al., « Reactjve depositjon of nitrides and oxides using a twin- cathode inverted cylindrical magnetron », Surface and Coatjngs Technology 133-134 (2000) 484-488.

Metalic mode Poisonned mode → Argon plasma → Nitrogen as reactjve gas → Titanium target → Formatjon of TiNx on target and substrate → Instability of the stoechiometric point

Stoechiometry (x=1)

  • PhD. Seminar - LE COZ T.

07/04/2016

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Employed technology

Reactjve sputuering

  • PhD. Seminar - LE COZ T.

→ Sputuering yield depends on the material

07/04/2016

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SLIDE 9
  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Geometry

Target Water cooling Magnet (NdFeB) Substrate Insulator 5 cm 10 cm Cathode :

  • Diameter : 5 cm
  • Length : 2*10 cm

Substrate :

  • Diameter : 2 mm
  • Grounded

Gas inlet Pumping → Two isolated targets for RF sputuering – we use DC sputuering

07/04/2016

Sofu iron

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SLIDE 10

07/04/2016

  • PhD. Seminar - LE COZ T.

10

Commercial magnetron

Magnetjc confjguratjon

Unit : T

→ 4 rings of 30 magnets → heterogeneity of the magnetjc fjeld → two racetracks per target → consumptjon of the targets : 30 % → Necessity of homogeneous magnetjc fjeld

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Magnetjc confjguratjon

→ Two ways to get a homogeneous magnetjc fjeld :

  • increase the diameter of the magnetjc rings
  • use a coil

Unit : T Magnetjc fjeld intensity on the target surface

0.038 T

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07/04/2016

  • PhD. Seminar - LE COZ T.

12

Commercial magnetron

Magnetjc confjguratjon

→ Two ways to get a homogeneous magnetjc fjeld :

  • increase the diameter of the magnetjc rings
  • use a coil

Unit : T Magnetjc fjeld intensity on the target surface

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Magnetjc confjguratjon

→ Electron leakage leading to the creeping and breaking of the wire

Atoms Ions

  • Sec. Therm. Total

6 12 18 24 30 36

VA = 0 V

Power (W) Species

Electrons

  • 30
  • 20
  • 10

10 20 30 100 200 300 400

Ofg-axis positjon (cm) Substrate temperature (°C) Species contributjons to the heat load of the substrate

→ Substrate to repulsive potentjal

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Magnetjc confjguratjon

→ Decrease of the substrate temperature → Modifjcatjon of the spatjal distributjon of the plasma

Schematjc of the depositjon chamber and pyrometric setup

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SLIDE 15

07/04/2016

  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Magnetjc confjguratjon

→ Plasma characterizatjon through Langmuir probe measurements. VA = 0 V VA = 30 V

Distributjon of the Langmuir characteristjcs within the magnetron Positjon along the cathode axis (cm) Probe potentjal (V) Current (mA) Positjon (cm) Probe potentjal (V) Current (mA)

→ Spatjal redistributjon of the plasma with the variatjons of the anode potentjal

Vf Vp Saturation ionique Ipb (mA) Vpb (V)

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Magnetjc confjguratjon

→ More energetjc electrons when polarizing and electron density slightly superior → Betuer ionizatjon but spatjal redistributjon of the plasma

No data because of a lack of collected current

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SLIDE 17

07/04/2016

  • PhD. Seminar - LE COZ T.

17

Commercial magnetron

Infmuence of the anode potentjal

C Ti Acier Acier Ti

VA = 0 V → Hysteresis shifued to higher nitrogen fmows → Grain size variatjon due to temperature → Difgusion of iron in the tjtanium coatjng

ASTAR pictures made by S. Grosso, SIMaP

VA = 0 V

EDX characterizatjon made by S. Grosso, SIMaP

VA = 30 V

1 2 3 4 5 6 200 400 600 800 1000 1200 1400 1600 Ti - N2↗ (30 V) Ti - N2↘ (30 V) Ti - N2↗ (0 V) Ti - N2↘ (0 V) Nitrogen fmow(sccm) Relatve intensity (a.u.)

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07/04/2016

  • PhD. Seminar - LE COZ T.

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→ Depositjon rate ≈ 60 nm/min → Depositjon profjle is changed due to plasma redistributjon

Cible Substrat

Heart-shaped pulverizatjon

Distance : D Cible Substrat Distance : D’

Commercial magnetron

Infmuence of the anode potentjal

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07/04/2016

  • PhD. Seminar - LE COZ T.

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3 6 9 12 15 50 100 150 200 250 300 350

mTorr 500 W

5 10 20 50 100

Target voltage (V) Current density (mA/cm

2)

1000 W

Ji ∝ (VT)12

4

2 4 6 8 10 12 50 100 150 200 250 LPM (mm) Pressure (mTorr)

→ JT α (VT)12 → Minimal turn-on pressure : 5 mTorr → Mean free path at 5 mTorr ≈ 25 mm = Distance cathode-target → Maximal operatjng power : 1000 W (by constructjon)

Alexandru Todoran, « Magnetron sputuering in inverted cylindrical confjguratjon : 3D depositoin on moving substrate », thèse 2014

Commercial magnetron

Operatjng parameters

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1 2 3 4 5 6 225 230 235 240 245 250 255 260 265 270 N2↗ (30 V) Nitrogen fmow (sccm) Cathode potentjal (V) 07/04/2016

  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Operatjng parameters

1 2 3 1 3 2 → More collisions due to the increase of species density leading to faster thermalizatjon → 1 : under-stoechiometric → 2 : stoechiometric → 3 : over-stoechiometric

1 2 3 4 5 6 200 400 600 800 1000 1200 1400 1600 Ti - N2↗ (30 V) Ti - N2↘ (30 V) N - N2↗ (30 V) Relatjve intensity (a.u.)

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Commercial magnetron

Intermediate conclusion

→ Necessity of homogeneous magnetjc fjeld → Control of the substrate temperature by polarizing auxiliary electrodes … → … which infmuences the plasma distributjon within the reactjon chamber → Low depositjon rate → Power input limited → Unstable conditjons for stoechiometric coatjngs

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Ugitech’s magnetron

Magnetjc confjguratjon

Unit : G → Non homogeneity of the magnetjc fjeld close to the target.

Ofg-axis positjon (cm) Bz (G)

150

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Ugitech’s magnetron

Magnetjc confjguratjon

0 0,8 1,8 4 5,5 9 10 11 13,5 17 19,5 21 22 24,5 25,5 28,2 29 30

Gas Gas Magnets

Racetracks Racetracks

  • 20 -15 -10
  • 5

5 10 15 20 20 40 60 80 100 120 140 160

0 V - 30 s Ofg-axis (cm) Substrate temperature (°C)

→ 5 racetracks → 6 electrons leakage zones → Target consumptjon: 36 %

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Ugitech’s magnetron

Operatjng parameters

→Higher sputuering for higher current →Increase of the ionizatjon rate

Hysteresis curves for difgerent target currents

→ Hysteresis for low nitrogen fmows

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Ugitech’s magnetron

Operatjng parameters

→ Mean depositjon rate : 100 nm/min against 60 nm/min in commercial cathode → Heterogeneous thickness → Polarizatjon infmuences spatjal plasma distributjon

Depositjon rate as a functjon of the positjon in the cathode

Commercial cathode Ugitech’s cathode

Ofg-axis positjon (cm)

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07/04/2016

  • PhD. Seminar - LE COZ T.

26

Ugitech’s magnetron

Titanium nitride coatjngs

→ Oxygen contaminatjon → Gold yellow is TiN → Blue is TiNxOy

N / Ti O/Ti 0.2 0.4 0.6 0.8 1 1.2 Ugi1– coté Ugi1 - Bosse Ugi1– centre

Ratjo of nitrogen and oxygen concentratjons with respect to the colors on the wire Coated wire made in reactjve mode under 30 V of polarizatjon, 5 min statjc depositjon

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07/04/2016

  • PhD. Seminar - LE COZ T.

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Ugitech’s magnetron

Intermediate conclusions

→ Necessity of homogeneous magnetjc fjeld → Control of the substrate temperature by polarizing auxiliary electrodes … → … which infmuences the plasma distributjon within the reactjon chamber → Depositjon rate greater than for the commercial cathode → Unknown limit of power input – grater than that for the commercial cathode → Unstable conditjons for stoechiometric coatjngs → Oxygen contaminatjon – Unknown origin

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Forthcoming work

→ Sizing of a coil → Study the infmuence of the diameter of the targets → Modeling of the sputuering process → Modeling of the gas dynamics → Find the origin of the oxygen contaminatjon → Ultjmately design a new optjmized magnetron