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Micro and nanostructural modification

of antimony selenide thin films

by laser and electron beam irradiation

Daugavpils University

The Faculty of Natural Sciences and Mathematics

G.Liberts' Innovative Microscopy Centre

1.

Introduction

Structure

A series of scientific publications

  • 62 pages
  • 38 figures
  • 4 tables
  • 1 appendix (39 pages)
  • 138 titles in References

Thesis

1. SbxSe100-x thin film etching rate in organic based solution e.g. amines depends on antimony percentage in compound. The crystalline region remains insoluble (V=0).

2. Laser and EB irradiation causes the crystallization of the Sb-Se amorphous films. Thin

film crystallization by laser beam starts from its surface, while the e-beam induced

crystallization begins at the metal/ChG boundary in the center of exposed spot,

extending radially and along the electrons propagation axis.

3. SbxSe100-x thin films laser irradiation followed by etching in organics based solution

leads to the relief formation, its profile characteristics depend on the composition.

4. Sb40Se60 thin films are suitable for EB lithography: the resolution of such a film

is ~ 1μm. Using the gray scale e-beam lithography it is possible to form relief in a

ChG thin film in a one step process (without etching stage).

5. The e-beam interaction with the ChG thin film phenomenologically

repeats the droplet impinging on a liquid surface.

Actuality & Application

of

by

Micro and nanostructural modification

antimony selenide thin films

laser and electron beam irradiation

Objectives

1. To study the etching process of as deposited, as well as

laser and electron beam exposed SbxSe100x thin films in

organic etchants.

2. To investigate the surface topography and the structure of

exposed and unexposed areas of the films SbxSe100-x

before and after the chemical etching.

3. To study the metal sublayer effect, as well as that of

electron beam parameters on surface modification under

e-beam irradiation.

4. To estimate the possibility to use Sb-Se thin films for the

electron beam lithography.

Aim

To investigate the Sb-Se thin film modification processes induced by laser and electron beam

Contents

2.

Methodology

Sample processing

Sb50Se50

SbxSe100-x

Metal

Sb40Se60

Glass

substrate

SbxSe100-x

Metal

Sb20Se80

Glass substrate

X-ray diffraction picture for as-deposited

Sb-Se thin films

Methods

• Electron Microscopy

• Confocal Optical Microscopy

• Atomic Force Microscopy

• Laser Spectroscopy

• X-ray Difractometry

• Energy Dispersive Spectrometry

• Electron BackScatter Kikuchi Diffraction (EBSD) methodology

• Optical Lithography

• Electron Lithography

Developed contactless method for in-situ real time monitoring of the

etching process

A schematic of the experimental wet-etching setup;

Alpha=0 in the case of using Leica TCSSPE microscope

The optical microscope image of irradiated Sb40Se60 thin films

Time dependent reflected signal during chemical etching of amorphous Sb-Se thin films

1. Introduction

2. Methodology

3. Research Results

4. Summary

3.

Research Results

EB induced changes

in Sb-Se thin films

Thesis 5.

The EB interaction with the ChG thin film phenomenologically repeats the droplet impinging on a liquid surface phenomenon.

Etching behavior of Sb-Se thin films

Thesis 1.

Amorphous SbxSe100-x‐ thin film etching rate in organic based solution e.g. amines depends on antimony percentage in compound. The crystalline region remains insoluble (υV=0).

Etching behavior of Sb-Se thin films

Thesis 1.

SbxSe100-x‐ thin film etching rate in organic based

solution e.g. amines depends on antimony percentage

in compound. The crystalline region remains insoluble (υV=0).

Etching behavior of Sb-Se thin films

Thesis 1.

У нас всегда есть возможность опровергнуть теорию, но, обратите внимание, мы никогда не можем доказать, что она правильна. Предположим, что вы выдвинули удачную гипотезу, рассчитали, к чему это ведет, и выяснили, что все ее следствия

подтверждаются экспериментально. Значит ли это, что ваша теория

правильна? Нет, просто-напросто это значит,

что вам не удалось ее опровергнуть.

SbxSe100-x‐ thin film etching rate in organic based solution e.g. amines depends on antimony percentage in compound. The crystalline region remains insoluble (υV=0).

Dependence of etching rate on at.% Sb

for SbхSe100-х thin films

R. Feinman

Time dependent reflected signal during etching of amorphous/crystallized and annealed (85 and 115°C) Sb20Se80 thin films

Sb40Se60

as an e-beam resist

Crystallization of Sb-Se thin films

Thesis 4.

Sb40Se60 thin films are suitable for EB lithography; its resolution is ~ 1μm. It is possible one step relief fabrication in ChG thin films (without etching stage) by gray scale EBL.

Thesis 2.

Laser and EB irradiation causes the crystallization of the Sb-‐Se amorphous films. Thin film crystallization by laser beam starts from its surface, while the e-‐beam induced crystallization begins at the metal/ChG boundary in the center of exposed spot, extending radially and along the electrons propagation axis.

Sb40Se60

as an e-beam resist

Thesis 4

Sb40Se60 thin films are suitable for EB lithography; its resolution is ~ 1μm. It is possible one step relief fabrication in ChG thin films (without etching stage) by gray scale EBL.

Crystallization of Sb-Se thin films

Sb40Se60

as an e-beam resist

Thesis 2.

Laser and EB irradiation causes the crystallization of the Sb-‐Se amorphous films. Thin film crystallization by laser beam starts from its surface, while the e-‐beam induced crystallization begins at the metal/ChG boundary in the center of exposed spot, extending radially and along the electrons propagation axis.

Thesis 4

Sb40Se60 thin films are suitable for EB lithography; its resolution is ~ 1μm. It is possible one step relief fabrication in ChG thin films (without etching stage) by gray scale EBL.

Sb40Se60

Se

Sb2O4

The distribution function of an average grain size

EBSD map of the e-beam irradiated area of Sb2Se3 thin film

The distribution function of the largest grain size

X-ray diffraction picture of Sb-Se thin films after laser treatment

Crystallization of Sb-Se thin films

Thesis 2.

Laser and EB irradiation causes the crystallization of the Sb-‐Se amorphous films. Thin film crystallization by laser beam starts from its surface, while the e-‐beam induced crystallization begins at the metal/ChG boundary in the center of exposed spot, extending radially and along the electrons propagation axis.

Relief formation

Thesis 3.

SbхSe100‐х thin films laser irradiation followed by etching in organics ‐based solution leads to the relief formation, its profile characteristics depend on the composition.

Sb

Se

50

Sb

Se

20

80

Sb

Se

40

60

4.

Summary

Conclusion

Acknowledgements

1. High etching selectivity of Sb-Se thin films in the organic

based solution.

2. The etching rate depends on the Sb percentage in compound.

3. E-beam or laser beam treatment leads to crystallization.

4. E-beam and laser beam can modify surface of ChG thin film.

5. It is possible to create the relief in Sb-Se thin films directly.

6. ChG thin film surface modification process by EB and

the drop collision with a free liquid surface

have a number of similarities.

Publications

8 papers in scientific journals

Conferences

4. Oksana Shiman, Vjačeslavs Gerbreders, Eriks Sledevskis, Andrejs Bulanovs

„Surface modification of SbSe thin films by laser irradiation and etching”, (2012)

doi: 10.2478/v1004701200055

5. O. Shiman, V. Gerbreders, E. Sledevskis, A. Bulanovs

“Selective Wet-Etching of Amorphous/Crystallized SbSe Thin Films”, (2012)

doi: 10.2478/v1004701200108

8. Oksana Šimane

„Excimer Laser and Electron Beam Irradiation

Effects in Sb40Se60 Thin Films”, (2012)

6. O. Shiman, V. Gerbreder, E. Sledevsky, A. Bulanov

“Electric conductivity of Sb/Se thin film microscale structures”, (2011)

doi: 10.2478/v1004701100069

7. O. Shiman, V. Gerbreders, E. Sledevskis, A. Bulanovs, V.Pashkevich

„Selective wet-etching of amorphous/crystallized Sb20Se80 thin films”, (2011)

http://www.waset.org/journals/waset/v75/v75147.pdf

1. Oksana Shiman, Vjaceslavs Gerbreders, Arnis Gulbis

"The interaction between electron beam and amorphous chalcogenide films”, (2012)

doi: 10.1016/j.jnoncrysol.2012.05.042

2. Oksana Shiman, Vjaceslavs Gerbreders, Eriks Sledevskis, Valfrids Paskevics

„Electron beam induced surface modification of amorphous Sb2Se3 thin film”, (2012)

doi: 10.1016/j.jnoncrysol.2012.02.013

3. Vadims Kolbjonoks, Vjačeslavs Gerbreders, Oksana Šimane

"Nanostructure formation on metal-chalcogenide surface using electron beam irradiation“, (2011)

doi:10.1016/j.jnoncrysol.2010.12.017.

  • 2012

1. The 11th International Conference on Global Research and Education, Budapest, Hungary

2. International Symposium on NonOxide and New Optical Glasses (XVIII ISNOG), StMalo, France

3. 14th International Materials, Methods and Technologies Symposium, Sunny Beach, Bulgaria

6 papers in conference proceedings

Proceedings of the International Scientific Conferences of Daugavpils University, (2009-2011):

  • 2011

4. 1st International Science Congress ISC2011, Indore, India

5. International Conference "Advanced Optical Materials and Devices" (AOMD7), Vilnius, Lithuania

6. International Conference for Academic Disciplines, Toronto, Ontario, Canada

7. SPIE Optics Optoelectronics 2011, Prague, Czech Republic

9. Oksana Shiman

„Wet-etching of SbSe thin films of stoichiometric compound and with excess selenium”

10. Oksana Šimane

„Stehiometriska sastāva Sb2Se3 plāno kārtiņiu elektrisko īpašbu izmaiņas fāžu pārejas amorfs/kristlisks stāvoklis gadījumā”

11. Oksana Šimane

„Optiskās, elektriskās īpašības un kristalizācijas procesi Sb-Se plānas kārtiņās”

Псковское университетское обозрениe (2009):

  • 2010

8. International Conference on Nanotechnology: Fundamentals and Applications, Ottawa, Canada

9. 17th International Symposium on NonOxide and New Optical Glasses (XVII ISNOG), Ningbo, China

10. International conference "Functional materials and nanotechnologies", Rīga, Latvia

12. Оксана Шимане

„Изменение электропроводности тонких пленок Sb2Se3 при кристаллизации”

Abstracts of The International Conference on Nanotechnology: Fundamentals and Applications (2010):

13. Oksana Simane, Vjaceslavs Gerbreders, Vadims Kolbjonoks

“Photo and heat stimulated changes in Sb/Se bilayered thin films”

14. Vadims Kolbjonoks, Vjaceslavs Gerbreders, Oksana Simane

"Nanostructure formation on metalchalcogenide surface using electron beam irradiation"

  • 2009

11. Международная научнопрактическая конференция, Pskov, Russia

12. 4th International Conference on Amorphous and Nanostructured Chalcogenides, Constanta, Romania

13-15. 25, 26 and 28th scientific conferences, Institute of Solid State Physics University of Latvia, Rīga, Latvija, 2009-2012.

16-19. 51-54th International Scientific Conferences of Daugavpils University, Daugavpils, Latvia, 2009-2012.

Oksana Šimane

The scientific adviser of the Doctoral Thesis:

Dr. phys. Vjaceslavs Gerbreders, DU IMC lead researcher

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