One-pot synthesis of amorphous high entropy Mo–C–N–O–S solids with ultradispersed Mo sites.

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Title: One-pot synthesis of amorphous high entropy Mo–C–N–O–S solids with ultradispersed Mo sites.
Authors: Ryaboshapka, Daria1 (AUTHOR) ryaboshapkada@gmail.com, Afanasiev, Pavel1 (AUTHOR)
Source: Journal of Materials Science. Dec2024, Vol. 59 Issue 45, p20982-20996. 15p.
Subjects: Light elements, Amorphous substances, Transmission electron microscopy, X-ray absorption, Mesoporous materials, Molybdenum
Abstract: Reaction of urea with ammonium heptamolybdate (HMA) at 550° in inert atmosphere leads to nanocrystalline molybdenum carbide Mo2C, whereas reaction of HMA with elemental sulfur gives MoS2 sulfide nanoparticles. Heating of sole urea in the same conditions is a well-known method to prepare C3N4. However, none of these phases is formed upon heating of a mixture of sulfur, HMA and urea, but the product has a complex high entropy Mo–C–N–O–S composition in which four light elements are randomly distributed around the Mo atoms. These solids remain amorphous and keep high surface area even at 550 °C, but disproportionate at 750 °C. The Mo–C–N–O–S solids prepared via this extremely simple one-pot synthesis route were studied by several techniques including X-ray absorption spectroscopy (XAS) and transmission electron microscopy (TEM). The materials are mesoporous and show promising HER activity in acidic conditions. Reaction mechanism leading to the mixed phase was studied by thermal analysis coupled with mass-spectrometry. XAS study demonstrated that Mo is surrounded by light atoms and has a small number of Mo neighbors. Remarkably, Mo species remain ultradispersed in the solids containing even 40 wt% of the metal. This study opens a new pathway toward high-entropy amorphous materials. [ABSTRACT FROM AUTHOR]
Copyright of Journal of Materials Science is the property of Springer Nature and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Data: One-pot synthesis of amorphous high entropy Mo–C–N–O–S solids with ultradispersed Mo sites.
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  Data: <searchLink fieldCode="AR" term="%22Ryaboshapka%2C+Daria%22">Ryaboshapka, Daria</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> ryaboshapkada@gmail.com</i><br /><searchLink fieldCode="AR" term="%22Afanasiev%2C+Pavel%22">Afanasiev, Pavel</searchLink><relatesTo>1</relatesTo> (AUTHOR)
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  Data: <searchLink fieldCode="JN" term="%22Journal+of+Materials+Science%22">Journal of Materials Science</searchLink>. Dec2024, Vol. 59 Issue 45, p20982-20996. 15p.
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  Data: <searchLink fieldCode="DE" term="%22Light+elements%22">Light elements</searchLink><br /><searchLink fieldCode="DE" term="%22Amorphous+substances%22">Amorphous substances</searchLink><br /><searchLink fieldCode="DE" term="%22Transmission+electron+microscopy%22">Transmission electron microscopy</searchLink><br /><searchLink fieldCode="DE" term="%22X-ray+absorption%22">X-ray absorption</searchLink><br /><searchLink fieldCode="DE" term="%22Mesoporous+materials%22">Mesoporous materials</searchLink><br /><searchLink fieldCode="DE" term="%22Molybdenum%22">Molybdenum</searchLink>
– Name: Abstract
  Label: Abstract
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  Data: Reaction of urea with ammonium heptamolybdate (HMA) at 550° in inert atmosphere leads to nanocrystalline molybdenum carbide Mo2C, whereas reaction of HMA with elemental sulfur gives MoS2 sulfide nanoparticles. Heating of sole urea in the same conditions is a well-known method to prepare C3N4. However, none of these phases is formed upon heating of a mixture of sulfur, HMA and urea, but the product has a complex high entropy Mo–C–N–O–S composition in which four light elements are randomly distributed around the Mo atoms. These solids remain amorphous and keep high surface area even at 550 °C, but disproportionate at 750 °C. The Mo–C–N–O–S solids prepared via this extremely simple one-pot synthesis route were studied by several techniques including X-ray absorption spectroscopy (XAS) and transmission electron microscopy (TEM). The materials are mesoporous and show promising HER activity in acidic conditions. Reaction mechanism leading to the mixed phase was studied by thermal analysis coupled with mass-spectrometry. XAS study demonstrated that Mo is surrounded by light atoms and has a small number of Mo neighbors. Remarkably, Mo species remain ultradispersed in the solids containing even 40 wt% of the metal. This study opens a new pathway toward high-entropy amorphous materials. [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Journal of Materials Science is the property of Springer Nature and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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      – Type: doi
        Value: 10.1007/s10853-024-10428-7
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      – Code: eng
        Text: English
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        PageCount: 15
        StartPage: 20982
    Subjects:
      – SubjectFull: Light elements
        Type: general
      – SubjectFull: Amorphous substances
        Type: general
      – SubjectFull: Transmission electron microscopy
        Type: general
      – SubjectFull: X-ray absorption
        Type: general
      – SubjectFull: Mesoporous materials
        Type: general
      – SubjectFull: Molybdenum
        Type: general
    Titles:
      – TitleFull: One-pot synthesis of amorphous high entropy Mo–C–N–O–S solids with ultradispersed Mo sites.
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            NameFull: Ryaboshapka, Daria
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            NameFull: Afanasiev, Pavel
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            – D: 01
              M: 12
              Text: Dec2024
              Type: published
              Y: 2024
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              Value: 45
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