Solid-state NMR study of crystallizing process of silicon nitride powder synthesized by the thermal decomposition method of imide

Hirotaka Fujimori, Koji Ioku, Seishi Goto, Tetsuo Yamada

Research output: Contribution to journalArticle

Abstract

Our recent investigation established a method for quantifying the amount of amorphous silicon nitride by 29Si MAS NMR technique, which involved the full relaxation of the 29Si nuclear spin system between pulses in order to make the signals proportional to the number of nuclei in each phase. In this work, solid-state NMR study of the crystallizing behavior of silicon nitride powder, synthesized by the thermal decomposition method of imide, has been attempted. Because the crystalline and amorphous phases of Si 3N 4 have different thermal expansion and oxidation susceptibilities, this difference strongly affects sinterability and the mechanical properties of the final sintered body. In view of the effects of crystalline vs. non-crystalline phases on sinterability and mechanical properties, it is crucial to establish a reliable method for measuring the quantities of α-, β-, and amorphous Si 3N 4 in the batches of Si 3N 4 powder before carrying out the sintering process. Moreover, because remains of hydrogenous products generally exist on the surface of the silicon nitride powder, this affects the characteristic of slurry and sinterability of the Si 3N 4 powder. Thus, the quantification of the amount of hydrogenous products in the silicon nitride powder is also required. According to 29Si MAS NMR spectra of silicon diimide (Si(NH) 2) during thermal decomposition at a series of temperatures, the crystalline phase increased as calcination temperatures increased. The integrated intensities of 1H MAS NMR spectra varied directly as specific surface areas. The bands near 1630 and 3300 cm -1 arising from adsorbed molecular water and the unknown band near 1400 cm -1 were observed in IR spectra. This result can be interpreted as indicating that there exists a proportional amount of compound consisting of hydrogen to specific surface area on the surface of silicon nitride powder, which was measured by 1H MAS NMR.

Original languageEnglish
Pages (from-to)132-136
Number of pages5
JournalNippon Seramikkusu Kyokai Gakujutsu Ronbunshi/Journal of the Ceramic Society of Japan
Volume109
Issue number1266
Publication statusPublished - 2001 Feb
Externally publishedYes

Fingerprint

Imides
imides
Silicon nitride
silicon nitrides
Powders
thermal decomposition
Pyrolysis
Nuclear magnetic resonance
solid state
nuclear magnetic resonance
Crystalline materials
Specific surface area
mechanical properties
Mechanical properties
Silicon
products
Amorphous silicon
nuclear spin
Calcination
roasting

Keywords

  • Amorphous
  • Crystallizing process
  • NMR
  • Quantitative analysis
  • Silicon nitride

ASJC Scopus subject areas

  • Ceramics and Composites

Cite this

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title = "Solid-state NMR study of crystallizing process of silicon nitride powder synthesized by the thermal decomposition method of imide",
abstract = "Our recent investigation established a method for quantifying the amount of amorphous silicon nitride by 29Si MAS NMR technique, which involved the full relaxation of the 29Si nuclear spin system between pulses in order to make the signals proportional to the number of nuclei in each phase. In this work, solid-state NMR study of the crystallizing behavior of silicon nitride powder, synthesized by the thermal decomposition method of imide, has been attempted. Because the crystalline and amorphous phases of Si 3N 4 have different thermal expansion and oxidation susceptibilities, this difference strongly affects sinterability and the mechanical properties of the final sintered body. In view of the effects of crystalline vs. non-crystalline phases on sinterability and mechanical properties, it is crucial to establish a reliable method for measuring the quantities of α-, β-, and amorphous Si 3N 4 in the batches of Si 3N 4 powder before carrying out the sintering process. Moreover, because remains of hydrogenous products generally exist on the surface of the silicon nitride powder, this affects the characteristic of slurry and sinterability of the Si 3N 4 powder. Thus, the quantification of the amount of hydrogenous products in the silicon nitride powder is also required. According to 29Si MAS NMR spectra of silicon diimide (Si(NH) 2) during thermal decomposition at a series of temperatures, the crystalline phase increased as calcination temperatures increased. The integrated intensities of 1H MAS NMR spectra varied directly as specific surface areas. The bands near 1630 and 3300 cm -1 arising from adsorbed molecular water and the unknown band near 1400 cm -1 were observed in IR spectra. This result can be interpreted as indicating that there exists a proportional amount of compound consisting of hydrogen to specific surface area on the surface of silicon nitride powder, which was measured by 1H MAS NMR.",
keywords = "Amorphous, Crystallizing process, NMR, Quantitative analysis, Silicon nitride",
author = "Hirotaka Fujimori and Koji Ioku and Seishi Goto and Tetsuo Yamada",
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AU - Fujimori, Hirotaka

AU - Ioku, Koji

AU - Goto, Seishi

AU - Yamada, Tetsuo

PY - 2001/2

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N2 - Our recent investigation established a method for quantifying the amount of amorphous silicon nitride by 29Si MAS NMR technique, which involved the full relaxation of the 29Si nuclear spin system between pulses in order to make the signals proportional to the number of nuclei in each phase. In this work, solid-state NMR study of the crystallizing behavior of silicon nitride powder, synthesized by the thermal decomposition method of imide, has been attempted. Because the crystalline and amorphous phases of Si 3N 4 have different thermal expansion and oxidation susceptibilities, this difference strongly affects sinterability and the mechanical properties of the final sintered body. In view of the effects of crystalline vs. non-crystalline phases on sinterability and mechanical properties, it is crucial to establish a reliable method for measuring the quantities of α-, β-, and amorphous Si 3N 4 in the batches of Si 3N 4 powder before carrying out the sintering process. Moreover, because remains of hydrogenous products generally exist on the surface of the silicon nitride powder, this affects the characteristic of slurry and sinterability of the Si 3N 4 powder. Thus, the quantification of the amount of hydrogenous products in the silicon nitride powder is also required. According to 29Si MAS NMR spectra of silicon diimide (Si(NH) 2) during thermal decomposition at a series of temperatures, the crystalline phase increased as calcination temperatures increased. The integrated intensities of 1H MAS NMR spectra varied directly as specific surface areas. The bands near 1630 and 3300 cm -1 arising from adsorbed molecular water and the unknown band near 1400 cm -1 were observed in IR spectra. This result can be interpreted as indicating that there exists a proportional amount of compound consisting of hydrogen to specific surface area on the surface of silicon nitride powder, which was measured by 1H MAS NMR.

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