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History of ALD: from lab research to industrial applications 
Beneq and ETU joint ALD laboratory opening seminar 15.11.2013 Riikka Puurunen (Dr.), Senior Scientist VTT Technical Research Centre of Finland
15/11/2013 2 
Riikka Puurunen, VTT, 15.11.2013 
Outline 
1. 
Very briefly about ALD (-ML) 
2. 
Suntola’s invention: from lab to production and beyond 
3. 
Aleskovskii, Kol’tsov and the Virtual project on the history of ALD 
4. 
Conclusion
15/11/2013 3 
Riikka Puurunen, VTT, 15.11.2013 
ALD: a chemical gas-phase technique for growing conformal (inorganic) material layers on solid substrates 
ALD cycle Substratebefore ALDStep 2 /4purgeStep 4 /4purgeStep 1 /4 Reactant AStep 3 /4Reactant B Reactant AReactant BBy-product 
From: Aarik et al., Thin Solid Films 340 (1999) 110, adapted with permission 
saturating, irreversible chemisorption reactions
15/11/2013 4 
Riikka Puurunen, VTT, 15.11.2013 
ALD, atomic layer deposition АСО, атомно-слоевое осаждение ≡ ML, molecular layering, МН, молекулярное наслаивание
15/11/2013 5 
Riikka Puurunen, VTT, 15.11.2013 
Many classes of materials have been studied by ALD: oxides, nitrides, sulfides, metals, … 
Source: review by Miikkulainen, Leskelä, Ritala, Puurunen, J. Appl. Phys. 113, 021301 (2013); http://dx.doi.org/10.1063/1.4757907 with >2000 references
15/11/2013 6 
Riikka Puurunen, VTT, 15.11.2013 
Many classes of materials have been studied by ALD: oxides, nitrides, sulfides, metals, … 
Source: review by Miikkulainen, Leskelä, Ritala, Puurunen, J. Appl. Phys. 113, 021301 (2013); http://dx.doi.org/10.1063/1.4757907 with >2000 references 
! 
Drozd
15/11/2013 7 
Riikka Puurunen, VTT, 15.11.2013 
TFEL displays - start 
Used with permission from Tuomo Suntola 
0.4 μm grown in 30 min from elements Zn and S
15/11/2013 8 
Riikka Puurunen, VTT, 15.11.2013 
FIN 52359, US 4 058 430, …M ethod for producing compound thin fims 
ALE Patent
15/11/2013 9 
Riikka Puurunen, VTT, 15.11.2013 
TFEL displays - structure 
 Production since ~1985 
Used with permission from Tuomo Suntola 
ZnS(Mn) from ZnCl2, H2S (MnCl2) 
ATO from AlCl3, TiCl4, H2O
15/11/2013 10 
Riikka Puurunen, VTT, 15.11.2013 
Used with permission from Jonas Sundqvist 
Metal-oxide-semiconductor field effect transistors (MOSFET) Dynamic random access memories (DRAM) 
DRAM 2004 
MOSFET 
2007
15/11/2013 11 
Riikka Puurunen, VTT, 15.11.2013 
Thin film ALD reactor technology: key to industrial success 
Solved for the TFEL production: 
 
Fast pulsing to grow thick films (>>100 nm) productively 
 
High-temperature valving with inert gas 
 
Large batch reactors 
 
… 
Finnish ALD equipment manufacturers have their roots in the TFEL display manufacturing  Fast, productive reactors
15/11/2013 12 
Riikka Puurunen, VTT, 15.11.2013 
TFEL displays - structure 
Used with permission from Tuomo Suntola
15/11/2013 13 
Riikka Puurunen, VTT, 15.11.2013 
Used with permission from Tuomo Suntola 
???
15/11/2013 14 
Riikka Puurunen, VTT, 15.11.2013 
Limit: year 1986
15/11/2013 15 
Riikka Puurunen, VTT, 15.11.2013
15/11/2013 16 
Riikka Puurunen, VTT, 15.11.2013 
Please join! Open until Dec 31 
Authors to be confirmed by Nov 20
15/11/2013 17 
Riikka Puurunen, VTT, 15.11.2013 
Many questions looking for answers 
 
What is the first public record of the invention of ALD in Russia? 
 
What is the Matrix hypothesis and how is it related to ALD? 
 
What kinds of thin film studies? 
 
Are there microelectronic applications? 
 
What kinds of reactors? 
 
Powders 
 
Thin films 
 
… other? 
 
What kind of catalysts? 
 
What kinds of sorbents? 
 
What other applications? 
 
How was it to do research with Aleskovskii & Koltsov? 
 
Is there ALD reactant development in Russia? 
 
ALD in industrial scale in Russia? 
 
Products? 
 
How and when did Russian scientists get to know of other ALD groups? 
 
Current ALD activities in Russia? 
 
...
15/11/2013 18 
Riikka Puurunen, VTT, 15.11.2013 
Conference: November 26-29, 1965, Leningrad 
TiCl4/H2O at 180C on silica 
ALD cycles since 1965
15/11/2013 19 
Riikka Puurunen, VTT, 15.11.2013 
Thin film studies since 1969 
Vacuum thin film ALD reactors 
SPbU 
Films, nanolaminates, alloys… Prof. Aleskovskii in 1974 predicted future microelectronics devise shrinkage and important role of ALD
15/11/2013 20 
Riikka Puurunen, VTT, 15.11.2013 
Particle coating knowhow & products 
From Hilovo 2012 presentation by Prof Malygin, used with permission 
Adsorbents to stabilize the device’s internal environment during storage and operation: P2O5 & VO3 POCl3/H2O, VOCl3/H2O 
Ceramics for X-ray tubes, ML to decrease sintering temperature: TiO2 & V2O5 from TiCl4/H2O, VOCl3/H2O 
Particle ML: Indicators, sorbents, catalysts, composite fillers, … 
SPb Technological Institute
15/11/2013 21 
Riikka Puurunen, VTT, 15.11.2013 
To conclude: 
 
Finnish ALD (ALE) 
 
Industry-initiated in 1974 
 
Production of TFEL displays already in mid-1980’s 
 
Tool manufacturers 
 
Russia has a rich history of ALD, however the details have been largely unknown to many 
 
Please participate in the Virtual project on the history of ALD: 
 
Help us to generate an overview of the Russian works to help us learn from them 
 
Participate in the poster and at Baltic ALD 2014 (Dec 31) 
 
”Open authorship” for the review article (Nov 20)
15/11/2013 22 
Riikka Puurunen, VTT, 15.11.2013 
Acknowledgements 
 
Dr. Tuomo Suntola (Espoo, Finland) 
 
Prof. Anatoly Malygin (St Peterburg State Technological Institute, Russia) 
 
Prof. Victor Drozd (St Petersburg State University, Russia) 
 
Dr. Yury Koshtyal (Ioffe institute, Russia) 
 
Dr. Aziz Abdulagatov (National Institute of Standards and Technology, USA) 
 
Dr. Jonas Sundqvist (Fraunhofer IPMS- CNT, Germany) 
 
… and all others who have helped in the Virtual Project on the History of ALD 
Thank you for your attention 
СПАСИБО ЗА ВНИМАНИЕ! 
ВОПРОСЫ?
15/11/2013 23 
Riikka Puurunen, VTT, 15.11.2013 
VTT creates business from technology

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History of ald riikka puurunen 15.11.2013 final

  • 1. History of ALD: from lab research to industrial applications Beneq and ETU joint ALD laboratory opening seminar 15.11.2013 Riikka Puurunen (Dr.), Senior Scientist VTT Technical Research Centre of Finland
  • 2. 15/11/2013 2 Riikka Puurunen, VTT, 15.11.2013 Outline 1. Very briefly about ALD (-ML) 2. Suntola’s invention: from lab to production and beyond 3. Aleskovskii, Kol’tsov and the Virtual project on the history of ALD 4. Conclusion
  • 3. 15/11/2013 3 Riikka Puurunen, VTT, 15.11.2013 ALD: a chemical gas-phase technique for growing conformal (inorganic) material layers on solid substrates ALD cycle Substratebefore ALDStep 2 /4purgeStep 4 /4purgeStep 1 /4 Reactant AStep 3 /4Reactant B Reactant AReactant BBy-product From: Aarik et al., Thin Solid Films 340 (1999) 110, adapted with permission saturating, irreversible chemisorption reactions
  • 4. 15/11/2013 4 Riikka Puurunen, VTT, 15.11.2013 ALD, atomic layer deposition АСО, атомно-слоевое осаждение ≡ ML, molecular layering, МН, молекулярное наслаивание
  • 5. 15/11/2013 5 Riikka Puurunen, VTT, 15.11.2013 Many classes of materials have been studied by ALD: oxides, nitrides, sulfides, metals, … Source: review by Miikkulainen, Leskelä, Ritala, Puurunen, J. Appl. Phys. 113, 021301 (2013); http://dx.doi.org/10.1063/1.4757907 with >2000 references
  • 6. 15/11/2013 6 Riikka Puurunen, VTT, 15.11.2013 Many classes of materials have been studied by ALD: oxides, nitrides, sulfides, metals, … Source: review by Miikkulainen, Leskelä, Ritala, Puurunen, J. Appl. Phys. 113, 021301 (2013); http://dx.doi.org/10.1063/1.4757907 with >2000 references ! Drozd
  • 7. 15/11/2013 7 Riikka Puurunen, VTT, 15.11.2013 TFEL displays - start Used with permission from Tuomo Suntola 0.4 μm grown in 30 min from elements Zn and S
  • 8. 15/11/2013 8 Riikka Puurunen, VTT, 15.11.2013 FIN 52359, US 4 058 430, …M ethod for producing compound thin fims ALE Patent
  • 9. 15/11/2013 9 Riikka Puurunen, VTT, 15.11.2013 TFEL displays - structure  Production since ~1985 Used with permission from Tuomo Suntola ZnS(Mn) from ZnCl2, H2S (MnCl2) ATO from AlCl3, TiCl4, H2O
  • 10. 15/11/2013 10 Riikka Puurunen, VTT, 15.11.2013 Used with permission from Jonas Sundqvist Metal-oxide-semiconductor field effect transistors (MOSFET) Dynamic random access memories (DRAM) DRAM 2004 MOSFET 2007
  • 11. 15/11/2013 11 Riikka Puurunen, VTT, 15.11.2013 Thin film ALD reactor technology: key to industrial success Solved for the TFEL production:  Fast pulsing to grow thick films (>>100 nm) productively  High-temperature valving with inert gas  Large batch reactors  … Finnish ALD equipment manufacturers have their roots in the TFEL display manufacturing  Fast, productive reactors
  • 12. 15/11/2013 12 Riikka Puurunen, VTT, 15.11.2013 TFEL displays - structure Used with permission from Tuomo Suntola
  • 13. 15/11/2013 13 Riikka Puurunen, VTT, 15.11.2013 Used with permission from Tuomo Suntola ???
  • 14. 15/11/2013 14 Riikka Puurunen, VTT, 15.11.2013 Limit: year 1986
  • 15. 15/11/2013 15 Riikka Puurunen, VTT, 15.11.2013
  • 16. 15/11/2013 16 Riikka Puurunen, VTT, 15.11.2013 Please join! Open until Dec 31 Authors to be confirmed by Nov 20
  • 17. 15/11/2013 17 Riikka Puurunen, VTT, 15.11.2013 Many questions looking for answers  What is the first public record of the invention of ALD in Russia?  What is the Matrix hypothesis and how is it related to ALD?  What kinds of thin film studies?  Are there microelectronic applications?  What kinds of reactors?  Powders  Thin films  … other?  What kind of catalysts?  What kinds of sorbents?  What other applications?  How was it to do research with Aleskovskii & Koltsov?  Is there ALD reactant development in Russia?  ALD in industrial scale in Russia?  Products?  How and when did Russian scientists get to know of other ALD groups?  Current ALD activities in Russia?  ...
  • 18. 15/11/2013 18 Riikka Puurunen, VTT, 15.11.2013 Conference: November 26-29, 1965, Leningrad TiCl4/H2O at 180C on silica ALD cycles since 1965
  • 19. 15/11/2013 19 Riikka Puurunen, VTT, 15.11.2013 Thin film studies since 1969 Vacuum thin film ALD reactors SPbU Films, nanolaminates, alloys… Prof. Aleskovskii in 1974 predicted future microelectronics devise shrinkage and important role of ALD
  • 20. 15/11/2013 20 Riikka Puurunen, VTT, 15.11.2013 Particle coating knowhow & products From Hilovo 2012 presentation by Prof Malygin, used with permission Adsorbents to stabilize the device’s internal environment during storage and operation: P2O5 & VO3 POCl3/H2O, VOCl3/H2O Ceramics for X-ray tubes, ML to decrease sintering temperature: TiO2 & V2O5 from TiCl4/H2O, VOCl3/H2O Particle ML: Indicators, sorbents, catalysts, composite fillers, … SPb Technological Institute
  • 21. 15/11/2013 21 Riikka Puurunen, VTT, 15.11.2013 To conclude:  Finnish ALD (ALE)  Industry-initiated in 1974  Production of TFEL displays already in mid-1980’s  Tool manufacturers  Russia has a rich history of ALD, however the details have been largely unknown to many  Please participate in the Virtual project on the history of ALD:  Help us to generate an overview of the Russian works to help us learn from them  Participate in the poster and at Baltic ALD 2014 (Dec 31)  ”Open authorship” for the review article (Nov 20)
  • 22. 15/11/2013 22 Riikka Puurunen, VTT, 15.11.2013 Acknowledgements  Dr. Tuomo Suntola (Espoo, Finland)  Prof. Anatoly Malygin (St Peterburg State Technological Institute, Russia)  Prof. Victor Drozd (St Petersburg State University, Russia)  Dr. Yury Koshtyal (Ioffe institute, Russia)  Dr. Aziz Abdulagatov (National Institute of Standards and Technology, USA)  Dr. Jonas Sundqvist (Fraunhofer IPMS- CNT, Germany)  … and all others who have helped in the Virtual Project on the History of ALD Thank you for your attention СПАСИБО ЗА ВНИМАНИЕ! ВОПРОСЫ?
  • 23. 15/11/2013 23 Riikka Puurunen, VTT, 15.11.2013 VTT creates business from technology