Thermodynamics of amorphous SiN(O)H dielectric films synthesized by plasma‐enhanced chemical vapor deposition

Chen, Jiewei; Niu, Min; Calvin, Jason; Asplund, Megan; King, Sean W.; Woodfield, Brian F.; Navrotsky, Alexandra

doi:10.1111/jace.15350

Title: Thermodynamics of amorphous SiN(O)H dielectric films synthesized by plasma‐enhanced chemical vapor deposition

Abstract

Abstract Thin films of amorphous Si NH (a‐Si NH ) and amorphous Si NOH (a‐Si NOH ) synthesized by plasma‐enhanced chemical vapor deposition ( PECVD ) are used extensively in the semiconductor industry, but little is known regarding their thermodynamic stability, and there are several long‐term reliability issues for these materials. To address the stability issues, a detailed thermodynamic investigation has been conducted on a series of a‐Si NH , and a‐Si NOH dielectric films. High‐temperature oxidative drop‐solution calorimetry in molten sodium molybdate solvent at 1075 K was utilized to determine the formation enthalpies from the elements and from crystalline counterparts/gaseous products. Together with entropy data derived from cryogenic heat capacity measurements, we confirmed that the incorporation of more hydrogen and oxygen leads to more negative enthalpies and Gibbs free energies of formation from elements. Coupled with FTIR structural analysis, the thermochemical data suggest that the Si–H ₂ chain structure and Si–O–Si bonding configurations provide the system with extra thermodynamic stability. However, the Gibbs free energies of formation from crystalline constituents and gaseous products are either positive or nearly zero, indicating that these amorphous films are not stable against decomposition, which may cause problems in high‐temperature applications.

Authors:

Chen, Jiewei ^[1]; Niu, Min ^[2];

^[3]; Asplund, Megan ^[3]; King, Sean W. ^[4]; Woodfield, Brian F. ^[3];

^[1]

Peter A. Rock Thermochemistry Laboratory and NEAT ORU University of California Davis Davis California
Peter A. Rock Thermochemistry Laboratory and NEAT ORU University of California Davis Davis California, State Key Laboratory for Mechanical Behavior of Materials Xi'an Jiaotong University Xi'an China
Department of Chemistry and Biochemistry Brigham Young University Provo Utah
Logic Technology Development Intel Corporation Hillsboro Oregon

Publication Date:: Fri Dec 01 00:00:00 EST 2017

Sponsoring Org.:: USDOE

OSTI Identifier:: 1411087

Grant/Contract Number:: DE‐SC0016446

Resource Type:: Publisher's Accepted Manuscript

Journal Name:: Journal of the American Ceramic Society

Additional Journal Information:: Journal Name: Journal of the American Ceramic Society Journal Volume: 101 Journal Issue: 5; Journal ID: ISSN 0002-7820

Publisher:: Wiley-Blackwell

Country of Publication:: United States

Language:: English

Citation Formats


                    Chen, Jiewei, Niu, Min, Calvin, Jason, Asplund, Megan, King, Sean W., Woodfield, Brian F., and Navrotsky, Alexandra. Thermodynamics of amorphous SiN(O)H dielectric films synthesized by plasma‐enhanced chemical vapor deposition.  United States: N. p., 2017. 
Web.  doi:10.1111/jace.15350.

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                    Chen, Jiewei, Niu, Min, Calvin, Jason, Asplund, Megan, King, Sean W., Woodfield, Brian F., & Navrotsky, Alexandra. Thermodynamics of amorphous SiN(O)H dielectric films synthesized by plasma‐enhanced chemical vapor deposition.  United States.  https://doi.org/10.1111/jace.15350

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                    Chen, Jiewei, Niu, Min, Calvin, Jason, Asplund, Megan, King, Sean W., Woodfield, Brian F., and Navrotsky, Alexandra. Fri .  
"Thermodynamics of amorphous SiN(O)H dielectric films synthesized by plasma‐enhanced chemical vapor deposition".  United States.  https://doi.org/10.1111/jace.15350.

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@article{osti_1411087,

  title        = {Thermodynamics of amorphous SiN(O)H dielectric films synthesized by plasma‐enhanced chemical vapor deposition},

  author       = {Chen, Jiewei and Niu, Min and Calvin, Jason and Asplund, Megan and King, Sean W. and Woodfield, Brian F. and Navrotsky, Alexandra},

  abstractNote = {Abstract Thin films of amorphous Si NH (a‐Si NH ) and amorphous Si NOH (a‐Si NOH ) synthesized by plasma‐enhanced chemical vapor deposition ( PECVD ) are used extensively in the semiconductor industry, but little is known regarding their thermodynamic stability, and there are several long‐term reliability issues for these materials. To address the stability issues, a detailed thermodynamic investigation has been conducted on a series of a‐Si NH , and a‐Si NOH dielectric films. High‐temperature oxidative drop‐solution calorimetry in molten sodium molybdate solvent at 1075 K was utilized to determine the formation enthalpies from the elements and from crystalline counterparts/gaseous products. Together with entropy data derived from cryogenic heat capacity measurements, we confirmed that the incorporation of more hydrogen and oxygen leads to more negative enthalpies and Gibbs free energies of formation from elements. Coupled with FTIR structural analysis, the thermochemical data suggest that the Si–H 2 chain structure and Si–O–Si bonding configurations provide the system with extra thermodynamic stability. However, the Gibbs free energies of formation from crystalline constituents and gaseous products are either positive or nearly zero, indicating that these amorphous films are not stable against decomposition, which may cause problems in high‐temperature applications.},

  doi          = {10.1111/jace.15350},

  journal      = {Journal of the American Ceramic Society},

  number       = 5,

  volume       = 101,

  place        = {United States},

  year         = {Fri Dec 01 00:00:00 EST 2017},

  month        = {Fri Dec 01 00:00:00 EST 2017}

}

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Title: Thermodynamics of amorphous SiN(O)H dielectric films synthesized by plasma‐enhanced chemical vapor deposition

Abstract

Citation Formats

Lattice vacancies responsible for the linear dependence of the low-temperature heat capacity of insulating materials journal, January 2015

Heat capacity of copper on the ITS-90 temperature scale using adiabatic calorimetry journal, October 2004

X-ray photoelectron spectroscopy measurement of the Schottky barrier at the SiC(N)/Cu interface journal, September 2011

Secondary phase inclusions in polycrystalline sheet silicon journal, September 2004

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Intrinsic stress effect on fracture toughness of plasma enhanced chemical vapor deposited SiNx:H films journal, June 2010

Growth and surface structure analysis of a new SiON single layer on SiC(0001) journal, October 2014

An improved technique for accurate heat capacity measurements on powdered samples using a commercial relaxation calorimeter journal, August 2011

Evidence for the formation of SiON glasses journal, April 1998

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Thermodynamic Stability of Low- k Amorphous SiOCH Dielectric Films journal, April 2016

Properties of Plasma-Deposited Silicon Nitride journal, January 1979

Network structure of a-SiO:H layers fabricated by plasma-enhanced chemical vapor deposition: Comparison with a-SiC:H layers journal, May 2016

Effect of gas composition on Si2N2O formation in the Si-C-N-O system journal, May 1991

Progress and new directions in high temperature calorimetry revisited journal, April 1997

Mechanical and thermophysical properties of PECVD oxynitride films measured by MEMS journal, November 2001

A method to extract absorption coefficient of thin films from transmission spectra of the films on thick substrates journal, April 2012

The Variation of Physical Properties of Plasma-Deposited Silicon Nitride and Oxynitride with Their Compositions journal, January 1984

Synthesis and characterization of silicon nitride whiskers journal, March 1990

Tunable Plasticity in Amorphous Silicon Carbide Films journal, July 2013

Characterization of Silicon-Oxynitride Films Deposited by Plasma-Enhanced CVD journal, January 1986

Improved resistive switching phenomena observed in SiN x -based resistive switching memory through oxygen doping process : Improved resistive switching phenomena observed in SiN journal, December 2013

Oxynitride glasses prepared from gels and melts journal, July 1983

Intrinsic stress fracture energy measurements for PECVD thin films in the SiOxCyNz:H system journal, July 2009

Oxynitride glasses and glass-ceramics journal, May 1980

Oxidation of silicon nitride prepared by plasma‐enhanced chemical vapor deposition at low temperature journal, October 1994

N-doped polymer-derived Si(N)OC: The role of the N-containing precursor journal, February 2015

Plasma‐enhanced growth, composition, and refractive index of silicon oxy‐nitride films journal, June 1995

Gas barrier properties of SiON films deposited by plasma enhanced chemical vapor deposition at low temperature as a function of the plasma process parameters journal, August 2013

Stability of hydrogen in silicon nitride films deposited by low-pressure and plasma enhanced chemical vapor deposition techniques journal, March 1989

Sinoite (Si 2 N 2 O); crystallization from EL chondrite impact melts journal, October 1997

Preparation of quaternary nitrogen-containing plasma films and their application to moisture sensors journal, August 1984

Formation of Si 2 N 2 O Microcrystalline Precipitates near the Quartz Crucible Wall Coated with Silicon Nitride in Cast-Grown Silicon journal, August 2013

Progress and new directions in high temperature calorimetry journal, January 1977

Optomechanical characterisation of compressively prestressed silicon oxynitride films deposited by plasma-enhanced chemical vapour deposition on silicon membranes journal, December 2004

Visible light emission from thin films containing Si, O, N, and H journal, September 1995

Analysis of Low-k Dielectric Thin Films on Thick Substrates by Transmission FTIR Spectroscopy journal, October 2014

Progress and New Directions in Calorimetry: A 2014 Perspective journal, October 2014

Dielectric Barrier, Etch Stop, and Metal Capping Materials for State of the Art and beyond Metal Interconnects journal, October 2014

Massive stress changes in plasma-enhanced chemical vapor deposited silicon nitride films on thermal cycling journal, July 2004

Minimization of dangling bond defects in hydrogenated silicon nitride dielectrics for thin film transistors (TFTs) journal, May 1998

Analysis of sub-stoichiometric hydrogenated silicon oxide films for surface passivation of crystalline silicon solar cells journal, September 2012

Numerical analysis of the formation of Si3N4 and Si2N2O during a directional solidification process in multicrystalline silicon for solar cells journal, April 2009

Fourier transform infrared spectroscopy investigation of chemical bonding in low-k a-SiC:H thin films journal, July 2011

Free energy model for the analysis of bonding in a ‐Si x N y H z alloys journal, May 1991

In situ study of amorphization and changes in coordination in Si 2 N 2 O at high pressure journal, April 2008

Fabrication of UV-transparent SixOyNz membranes with a low frequency PECVD reactor journal, April 2002

Comparative investigation of hydrogen bonding in silicon based PECVD grown dielectrics for optical waveguides journal, June 2004

Study of the mechanical and structural properties of silicon oxynitride films for optical applications journal, July 2006

Hydrogen incorporation in silicon (oxy)nitride thin films journal, November 1988

The high‐pressure behavior of α‐quartz, oxynitride, and nitride structures journal, January 1981

Properties of Si[sub x]O[sub y]N[sub z] Films on Si journal, January 1968

Lattice vacancies responsible for the linear dependence of the low-temperature heat capacity of insulating materials
journal, January 2015

Heat capacity of copper on the ITS-90 temperature scale using adiabatic calorimetry
journal, October 2004

X-ray photoelectron spectroscopy measurement of the Schottky barrier at the SiC(N)/Cu interface
journal, September 2011

Secondary phase inclusions in polycrystalline sheet silicon
journal, September 2004

Critical phenomena at the antiferromagnetic transition in MnO
journal, September 1999

Hydrogen bonding configurations in silicon nitride films prepared by plasma‐enhanced deposition
journal, July 1985

Intrinsic stress effect on fracture toughness of plasma enhanced chemical vapor deposited SiNx:H films
journal, June 2010

Growth and surface structure analysis of a new SiON single layer on SiC(0001)
journal, October 2014

An improved technique for accurate heat capacity measurements on powdered samples using a commercial relaxation calorimeter
journal, August 2011

Evidence for the formation of SiON glasses
journal, April 1998

Thermal dissociation process of hydrogen atoms in plasma-enhanced chemical vapor deposited silicon nitride films
journal, November 1998

Nuclear reaction analysis for H, Li, Be, B, C, N, O and F with an RBS check
journal, March 2016

Oxynitride Glasses
journal, August 1986

Plasma‐enhanced growth and composition of silicon oxynitride films
journal, October 1986

Thermal Expansion and Atomic Structure of Amorphous Silicon Nitride Thin Films
journal, October 2003

Enhanced Interfacial Adhesion and Osteogenesis for Rapid “Bone-like” Biomineralization by PECVD-Based Silicon Oxynitride Overlays
journal, July 2015

In-Situ Reactive Synthesis of Si2N2O Ceramics and Its Properties
journal, August 2012

Specific Heats at Low Temperatures
book, January 1966

Discussion on device structures and hermetic encapsulation for SiO _x random access memory operation in air
journal, October 2014

Thermally induced damages of PECVD SiN _x thin films
journal, August 2011

Solubility of Si3N4 in Liquid SiO2
journal, January 2002

Silicon oxynitride films deposited by reactive high power impulse magnetron sputtering using nitrous oxide as a single-source precursor
journal, September 2015

Thermodynamic Stability of Low- k Amorphous SiOCH Dielectric Films
journal, April 2016

Properties of Plasma-Deposited Silicon Nitride
journal, January 1979

Network structure of a-SiO:H layers fabricated by plasma-enhanced chemical vapor deposition: Comparison with a-SiC:H layers
journal, May 2016

Effect of gas composition on Si2N2O formation in the Si-C-N-O system
journal, May 1991

Progress and new directions in high temperature calorimetry revisited
journal, April 1997

Mechanical and thermophysical properties of PECVD oxynitride films measured by MEMS
journal, November 2001

A method to extract absorption coefficient of thin films from transmission spectra of the films on thick substrates
journal, April 2012

The Variation of Physical Properties of Plasma-Deposited Silicon Nitride and Oxynitride with Their Compositions
journal, January 1984

Synthesis and characterization of silicon nitride whiskers
journal, March 1990

Tunable Plasticity in Amorphous Silicon Carbide Films
journal, July 2013

Characterization of Silicon-Oxynitride Films Deposited by Plasma-Enhanced CVD
journal, January 1986

Improved resistive switching phenomena observed in SiN _x -based resistive switching memory through oxygen doping process : Improved resistive switching phenomena observed in SiN
journal, December 2013

Oxynitride glasses prepared from gels and melts
journal, July 1983

Intrinsic stress fracture energy measurements for PECVD thin films in the SiOxCyNz:H system
journal, July 2009

Oxynitride glasses and glass-ceramics
journal, May 1980

Oxidation of silicon nitride prepared by plasma‐enhanced chemical vapor deposition at low temperature
journal, October 1994

N-doped polymer-derived Si(N)OC: The role of the N-containing precursor
journal, February 2015

Plasma‐enhanced growth, composition, and refractive index of silicon oxy‐nitride films
journal, June 1995

Gas barrier properties of SiON films deposited by plasma enhanced chemical vapor deposition at low temperature as a function of the plasma process parameters
journal, August 2013

Stability of hydrogen in silicon nitride films deposited by low-pressure and plasma enhanced chemical vapor deposition techniques
journal, March 1989

Sinoite (Si ₂ N ₂ O); crystallization from EL chondrite impact melts
journal, October 1997

Preparation of quaternary nitrogen-containing plasma films and their application to moisture sensors
journal, August 1984

Formation of Si ₂ N ₂ O Microcrystalline Precipitates near the Quartz Crucible Wall Coated with Silicon Nitride in Cast-Grown Silicon
journal, August 2013

Progress and new directions in high temperature calorimetry
journal, January 1977

Optomechanical characterisation of compressively prestressed silicon oxynitride films deposited by plasma-enhanced chemical vapour deposition on silicon membranes
journal, December 2004

Visible light emission from thin films containing Si, O, N, and H
journal, September 1995

Analysis of Low-k Dielectric Thin Films on Thick Substrates by Transmission FTIR Spectroscopy
journal, October 2014

Progress and New Directions in Calorimetry: A 2014 Perspective
journal, October 2014

Dielectric Barrier, Etch Stop, and Metal Capping Materials for State of the Art and beyond Metal Interconnects
journal, October 2014

Massive stress changes in plasma-enhanced chemical vapor deposited silicon nitride films on thermal cycling
journal, July 2004

Minimization of dangling bond defects in hydrogenated silicon nitride dielectrics for thin film transistors (TFTs)
journal, May 1998

Analysis of sub-stoichiometric hydrogenated silicon oxide films for surface passivation of crystalline silicon solar cells
journal, September 2012

Numerical analysis of the formation of Si3N4 and Si2N2O during a directional solidification process in multicrystalline silicon for solar cells
journal, April 2009

Fourier transform infrared spectroscopy investigation of chemical bonding in low-k a-SiC:H thin films
journal, July 2011

Free energy model for the analysis of bonding in a ‐Si _x N _y H _z alloys
journal, May 1991

In situ study of amorphization and changes in coordination in ${Si}_{2} N_{2} O$ at high pressure
journal, April 2008

Fabrication of UV-transparent SixOyNz membranes with a low frequency PECVD reactor
journal, April 2002

Comparative investigation of hydrogen bonding in silicon based PECVD grown dielectrics for optical waveguides
journal, June 2004

Study of the mechanical and structural properties of silicon oxynitride films for optical applications
journal, July 2006

Hydrogen incorporation in silicon (oxy)nitride thin films
journal, November 1988

The high‐pressure behavior of α‐quartz, oxynitride, and nitride structures
journal, January 1981

Properties of Si[sub x]O[sub y]N[sub z] Films on Si
journal, January 1968