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Alexane VITAL Submicrometric structured silicon surfaces obtained from polymer blend film by silica replication and cryogenic plasma etching Pillars 200 nm PESM 2014 Thomas TILLOCHER, Rémi DUSSART, Marylène VAYER, Christophe SINTUREL

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Page 1: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Alexane VITAL

Submicrometric structured silicon surfaces obtained from polymer blend film

by silica replication and cryogenic plasma etching

Pillars 200 nm

PESM

2014

Thomas TILLOCHER, Rémi DUSSART, Marylène VAYER, Christophe SINTUREL

Page 2: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

PESM

2014

Context

The photolithography is generally used to realize

mask for plasma etching in the CMOS technology.

However, this step is limited for small size.

Develop nanostructured surfaces

Different solutions:

Block copolymer film Homopolymer blend film

+ E-beam lithography

2/16

Page 3: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Blending of two homopolymers :

In bulk :

phase separation at

macroscopic scale

PESM

2014

Elaboration of polymer mask

Selective extraction of one component :

Selective extraction of

the minor component

Selective extraction of

the major component

In thin film : phase separation at nanometric or

submicrometric scale

Laterally phase

separated system Stratified system

Homogeneous system

Conditions:

Incompatibility of the two polymers

Surface energy of the polymers

Interaction between the polymer and the surface

3/16

Page 4: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Goal Develop nanostructured silicon surfaces by cryogenic plasma etching.

PESM

2014

To achieve this goal : 2 ways

Silica mask

Porous

polymer

mask

Thin film of polymers blend

Etched

surface

Replication of

selectively extracted

polymer film

Etched surface

Etched silicon surface 4/16

Page 5: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Elaboration of continuous polymer mask

Homopolymers

blend in solution Spin Coating

AFM images

PS

PLA

PESM

2014 Selective extraction of the minor

component

Solvent

evaporation

5/16

Page 6: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Selective extraction of the major

component

Elaboration of discrete polymer mask

Homopolymers

blend in solution Spin Coating

AFM images

PS

PLA

PESM

2014

Important parameter : Concentration allows to modify domains size

Solvent

evaporation

6/16

Page 7: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Preparation of continuous silica mask

Solution of silica

precursor is deposited Calcination After selective

extraction of the major

component

PESM

2014

Silica mask 200 nm

Discrete polymer film

7/16

Page 8: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Calcination Solution of silica

precursor is deposited

Selective extraction of

the minor component

PESM

2014

Preparation of discrete silica mask

Important parameter :

Concentration of silica precursor allows to

modify the filling ratio

Silica mask 200 nm

Continuous polymer film

8/16

Page 9: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Cryogenic Plasma Etching

Equipement :

Alcatel 601E

The standard cryogenic process allows to obtain high etch rates with

smooth sidewalls

In a standard process, silicon substrate is :

cooled down at a cryogenic temperature (-120°C)

exposed to a monocyclic SF6/O2 plasma

Passivation layer : SiOxFy

prevents lateral etching and so promotes vertical etching

is stable only at low temperature and is desorbed when

heated to room temperature

PESM

2014

9/16

Page 10: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Plasma etching (45 s)

ERSi : 1.6 µm.min-1

Cryogenic Plasma Etching

with continuous polymer mask

After selective extraction

of the minor component

PESM

2014

Depth : 800 nm

Cylindrical holes 1 µm

-120°C

10/16

Page 11: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Cylindrical holes 200 nm

Cryogenic Plasma Etching

with continuous silica mask

After calcination

PESM

2014

ERSi : 1.6 µm.min-1

Depth : 800 nm

Plasma etching (45 s)

-120°C

11/16

Page 12: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Concentration influence of

polymer solution The concentration of polymer solution is divided by two :

Cylindrical holes 200 nm

Holes size : 250 nm

Cylindrical holes 200 nm

Holes size : 500 nm

PESM

2014

20 mg.mL-1 10 mg.mL-1

Thickness of mask = 100 nm Thickness of mask = 50 nm

Etch holes with the same : Depth : 800 nm

ERSi : 1.6 µm.min-1

12/16

Page 13: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Influence of the choice of

extracted component During the preparation of the polymer film, selective extraction of the minor

component.

ERSi : 1.9 µm.min-1

Height : 1 µm

Pillars 200 nm

PESM

2014

After calcination

Height = 100 nm

Silica mask 200 nm

Plasma etching (45 s)

-120°C

13/16

Page 14: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

During the step of replication, lower concentration of the silica precursor

solution = 0.10 M

Silica bowls 200 nm

After calcination

Height for the edge = 100 nm

ERSi : 1.9 µm.min-1

Height : 1 µm

Vertical tubes 200 nm

Concentration influence of

silica precursor solution

PESM

2014

Height for the center = 20 nm

Plasma etching (45 s) -120°C

14/16

Page 15: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Conclusion

A wide range of etched structures can be prepared with such procedures.

Vertical tubes 200 nm

15/16 PESM

2014

Different silicon structures are obtained:

Elaboration of continuous or discrete masks:

Polymer mask

Silica mask

Cylindrical holes

Pillars

Tubes hollow in the upper part

Page 16: Submicrometric structured silicon surfaces obtained from …pesm2014.insight-outside.fr/presentations/Session3-4... · 2014. 6. 13. · Alexane VITAL Submicrometric structured silicon

Thank you for your

attention

Alexane VITAL 16 P

ESM

2014

16/16