DE10136499A1 - Process for changing the structure of silicon nitride ceramics comprises changing the process parameters - Google Patents

Process for changing the structure of silicon nitride ceramics comprises changing the process parameters

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DE10136499A1
DE10136499A1 DE2001136499 DE10136499A DE10136499A1 DE 10136499 A1 DE10136499 A1 DE 10136499A1 DE 2001136499 DE2001136499 DE 2001136499 DE 10136499 A DE10136499 A DE 10136499A DE 10136499 A1 DE10136499 A1 DE 10136499A1
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final structure
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sintering process
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Hans-Joachim Kleebe
Wolfgang Lehner
Guenter Ziegler
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    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract

Process for changing the structure of Si3N4 ceramics comprises changing the process parameters.

Description

Stand der TechnikState of the art

Im Gegensatz zu dem hier beschriebenen Verfahrensweg, verfolgten die bisher in der Literatur beschriebenen Verfahren zur Veränderung des Si3N4-Endgefüges folgende Ansätze (Abb. 1):

  • a) Die Beeinflussung des Si3N4-Endgefüges kann durch Variation der Ausgangspulver erzielt werden. In diesem Zusammenhang wiesen Ziegler et al.1 nach, dass eine hohe α-Si3N4-Konzentration im Ausgangspulver die Bildung eines bimodalen Gefüges fördert, wobei der durchschnittliche Streckungsgrad der β-Si3N4-Körner vom α-β-Verhältnis im Si3N4-Ausgangspulver abhängig ist2,3,4. Eine geschickte Dotierung sehr feiner β-Si3N4- Pulver mit nadelförmigen β-Si3N4-Kristalliten verändert nach Mitomo et al.5 sowohl die Anzahl großer, langgestreckter β-Si3N4-Körner im Endgefüge als auch deren Streckungsgrad. Beobachtet wurde in diesem Zusammenhang auch ein anisotropes Kornwachstum während des Sintervorganges, welches die Bildung langgestreckter β-Si3N4-Körner fördert6.
  • b) Eine weitere Möglichkeit der Gefügebeeinflussung von Si3N4 ist durch Variation von Temperatur und Haltezeit oberhalb 1750°C gegeben3,7. Durch Auslagerung bei Temperaturen oberhalb 1750°C wird nur das Wachstum großer langgestreckter Körner gefördert (Ostwaldreifung). Der Feinanteil bleibt im Gegensatz zu der im vorliegenden Patentantrag neuen Methode jedoch relativ unberührt.
  • c) Die Zugabe externer Keime stellt eine teuere Lösung zur Gefügevariation von Si3N4- Keramiken, da nur in (001)-Richtung orientierte β-Keime zu großen langgestreckten Keimen heranwachsen können und diese nur sehr begrenzt verfügbar sind.
In contrast to the process described here, the processes for changing the final Si 3 N 4 structure previously described in the literature pursued the following approaches ( Fig. 1):
  • a) The Si 3 N 4 final structure can be influenced by varying the starting powder. In this context, Ziegler et al. 1 after that a high α-Si 3 N 4 concentration in the starting powder promotes the formation of a bimodal structure, the average degree of stretching of the β-Si 3 N 4 grains depending on the α-β ratio in the Si 3 N 4 starting powder is 2,3,4 . A clever doping of very fine β-Si 3 N 4 powder with acicular β-Si 3 N 4 crystallites changed according to Mitomo et al. 5 both the number of large, elongated β-Si 3 N 4 grains in the final structure and their degree of stretching. Anisotropic grain growth during the sintering process was also observed in this connection, which promotes the formation of elongated β-Si 3 N 4 grains 6 .
  • b) A further possibility of influencing the structure of Si 3 N 4 is given by varying the temperature and holding time above 1750 ° C. 3.7 . By aging at temperatures above 1750 ° C, only the growth of large elongated grains is promoted (Ostwald maturation). In contrast to the new method in the present patent application, the fine fraction remains relatively unaffected.
  • c) The addition of external nuclei represents an expensive solution for the structure variation of Si 3 N 4 ceramics, since only in the (001) direction oriented β nuclei can grow into large elongated nuclei and these are only available to a very limited extent.

Beschreibung des VerfahrensDescription of the procedure

Im vorliegenden Patentantrag wird u. a. Variation der Aufheizrate der Effekt der unterschiedlichen Zeitabhängigkeit der Grenzflächenreaktion am α-Si3N4-Korn und der Diffusion durch die Sekundärphase ausgenutzt. Eine reduzierte Aufheizrate bewirkt eine erhöhte Anzahl lokaler Übersättigungen in der Schmelze und ein Ansteigen der Keimbildungsrate. Damit ist es möglich, Keimbildungsprozesse im Si3N4 zu initiieren und die Anzahl wachstumsfähiger Keime im Gefüge zu erhöhen, wodurch sich ein feinkörnigeres Endgefüge erzielen lässt. Verstärkt wird dieser Effekt durch das Einfügen einer zusätzlichen Haltezeit im Frühstadium der Verdichtung (1400-1700°C). In the present patent application, the effect of the different time dependency of the interface reaction on the α-Si 3 N 4 grain and the diffusion through the secondary phase is used, inter alia, by varying the heating rate. A reduced heating rate causes an increased number of local supersaturations in the melt and an increase in the nucleation rate. This makes it possible to initiate nucleation processes in Si 3 N 4 and to increase the number of growth-capable nuclei in the structure, as a result of which a finer-grained final structure can be achieved. This effect is reinforced by the addition of an additional holding time in the early stage of compression (1400-1700 ° C).

Durch zusätzliche Druckerhöhung im Frühstadium der Verdichtung kann die Anzahl großer langgestreckter β-Si3N4-Körner im Endgefüge gesteigert an. Mit der Verknüpfung der Variation der Prozeßparameter (Aufheizrate, Haltezeit und Druckerhöhung) lassen sich sowohl der Feinanteil als auch die Anzahl großer langgestreckter Körner im Si3N4-Endgefüge gezielt einstellen.


The number of large elongated β-Si 3 N 4 grains in the final structure can be increased by additional pressure increase in the early stage of compression. By linking the variation of the process parameters (heating rate, holding time and pressure increase), both the fine fraction and the number of large elongated grains in the final Si 3 N 4 structure can be set.


Im Vergleich zu den bisherigen Arbeiten ist es durch den hier vorgestellten neuartigen Ansatz gelungen, ausschließlich durch die Variation der Sinterparameter (t, T, p-Programm) im Frühstadium der Verdichtung (1400-1700°C) an identisch dotierten Grünkörpern keimbildende Vorgänge zu initiieren. Dies hat denselben Effekt wie die Zugabe einer Vielzahl kleiner externer β-Körner und kann gezielt zur Gefügeveränderung in Siliciumnitridkeramiken genutzt werden. Die Variation der Anzahl wachstumsfähiger β-Si3N4-Kristallite, ausgehend von ein und demselben Grünkörper, gelang unabhängig von der verwendeten Additivzusammensetzung. In comparison to previous work, the novel approach presented here succeeded in initiating nucleation processes on identically doped green bodies solely by varying the sintering parameters (t, T, p program) in the early stage of compaction (1400-1700 ° C) , This has the same effect as the addition of a large number of small external β-grains and can be used specifically to change the structure of silicon nitride ceramics. The variation in the number of growth-capable β-Si 3 N 4 crystallites, starting from one and the same green body, was achieved independently of the additive composition used.

Der Vorteil des hier vorgestellten neuartigen Verfahrens ist, im Vergleich zu den bisherigen Ansätzen, dass ausgehend von ein und demselben Grünkörper je nach Anforderungsprofil das jeweilige Endgefüge gezielt - ausschließlich durch Variation der Sinterparamter - eingestellt werden kann. The advantage of the new method presented here is compared to the previous ones Approaches that starting from one and the same green body depending on the requirement profile The respective final structure is set specifically - only by varying the sintering parameters can be.

Beispiel 1example 1 Einstellung eines feinkörnigen EndgefügesSetting a fine-grained final structure

Durch Einstellen einer geringeren Aufheizgeschwindigkeit wird die Anzahl lokaler Übersättigungen in der Schmelze erhöht. Dadurch steigt die Keimbildungswahrscheinlichkeit stark an. Damit ist es möglich, Si3N4-Keimbildungsprozesse zu initiieren und die Anzahl wachstumsfähiger Keime im Endgefüge zu erhöhen, wodurch ein feinkörnigeres Endgefüge eingestellt werden kann. By setting a lower heating rate, the number of local supersaturations in the melt is increased. This greatly increases the probability of nucleation. This makes it possible to initiate Si 3 N 4 nucleation processes and to increase the number of viable nuclei in the final structure, which means that a finer-grained final structure can be set.

Dieser Effekt kann durch das Einfügen einer zusätzlichen Haltezeit im Frühstadium der Verdichtung (1400-1700°C) verstärkt werden. This effect can be achieved by inserting an additional holding time in the early stages of the Compression (1400-1700 ° C) to be reinforced.

Beispiel 2Example 2 Einstellung eines feinkörnigen Endgefüges mit großen langgestreckten β-Si3N4-KörnernSetting of a fine-grained final structure with large elongated β-Si 3 N 4 grains

Durch zusätzliche Druckerhöhung im Frühstadium der Verdichtung kann die Anzahl großer langgestreckter β-Si3N4-Körner im Endgefüge gesteigert an. Mit der Verknüpfung der Variation der Prozeßparameter (Aufheizrate, Haltezeit und Druckerhöhung) lassen sich sowohl der Feinanteil als auch die Anzahl langgestreckter Körner im Si3N4-Endgefüge gezielt einstellen. Literatur zum Stand der Technik 1 Ziegler, J. Heinrich and G. Wötting,. "Relationship Between Processing, Microstructure and Properties of Dense and Reaction-Bonded Silicon Nitride", J. Mater. Sci., 22 (1987) 3041-86.
2 G. Wötting und G. Ziegler, "Dichtes Siliciumnitrid, II: Einflussfaktoren bei der Herstellung und Gefügeeigenschaften", Sprechsaal, 122 (1989) 45-57.
3 M. Krämer, "Untersuchungen zur Wachstumskinetik von β-Si3N4 in Keramiken und Oxynitridgläsern", Dissertation, Universität Stuttgart, (1991).
4 W. Dreßler, "Gefügeentwicklung und mechanische Eigenschaften von Si3N4-Keramiken", Diss., Universität Stuttgart (1993).
5 M. Mitomo, N. Yang, Y. Kishi and Y. Bando, "Influence of Powder Characteristics on Gas- Pressure Sintering of Si3N4", J. Mater. Sci. 23 (1988) 3412-19.
6 M. Hermann, H. Keßler und S. Heß, "Einfluss der Phasentransformation des Si3N4 und die Gefügeentwicklung", VII. Arbeitstagung Festkörperchemie und Keramik, Tagungsband (1988) 161-63.
7 L. Iskoe, F. F. Lange, "Development of Microstructure And Mechanical Properties During Hot Pressing of Si3N4", Ceramic Microstructures '76, With Emphasis on Energy Related Applications, (1976) 669-78. The number of large elongated β-Si 3 N 4 grains in the final structure can be increased by additional pressure increase in the early stage of compression. By linking the variation of the process parameters (heating rate, holding time and pressure increase), both the fine fraction and the number of elongated grains in the Si 3 N 4 final structure can be set in a targeted manner. Literature related to the state of the art 1 Ziegler, J. Heinrich and G. Wötting ,. "Relationship Between Processing, Microstructure and Properties of Dense and Reaction-Bonded Silicon Nitride", J. Mater. Sci., 22 (1987) 3041-86.
2 G. Wötting and G. Ziegler, "Dense Silicon Nitride, II: Factors Influencing Production and Structural Properties", at the conference hall, 122 (1989) 45-57.
3 M. Krämer, "Studies on the growth kinetics of β-Si 3 N 4 in ceramics and oxynitride glasses", dissertation, University of Stuttgart, (1991).
4 W. Dreßler, "Structure development and mechanical properties of Si 3 N 4 ceramics", Diss., University of Stuttgart (1993).
5 M. Mitomo, N. Yang, Y. Kishi and Y. Bando, "Influence of Powder Characteristics on Gas-Pressure Sintering of Si 3 N 4 ", J. Mater. Sci. 23 (1988) 3412-19.
6 M. Hermann, H. Keßler and S. Heß, "Influence of the phase transformation of Si 3 N 4 and the development of the microstructure", VII. Workshop Solid State Chemistry and Ceramics, conference volume (1988) 161-63.
7 L. Iskoe, FF Lange, "Development of Microstructure And Mechanical Properties During Hot Pressing of Si 3 N 4 ", Ceramic Microstructures '76, With Emphasis on Energy Related Applications, (1976) 669-78.

Claims (9)

1. Verfahren zur gezielten Veränderung des Gefüges von Si3N4-Keramiken, dadurch gekennzeichnet, dass die Prozessparameter verändert werden. 1. Process for the targeted change of the structure of Si 3 N 4 ceramics, characterized in that the process parameters are changed. 2. Das in Anspruch 1 beschriebene Verfahren, dadurch gekennzeichnet, dass es unabhängig vom gewählten Additivsystem ist. 2. The method described in claim 1, characterized, that it is independent of the additive system chosen. 3. Das in den Ansprüchen 1-2 beschriebene Verfahren, dadurch gekennzeichnet, dass nur durch Variation der Prozessparameter im Frühstadium der Verdichtung (Temperaturbereich 1400-1700°C), das Si3N4-Endgefüge beeinflußt wird. 3. The method described in claims 1-2, characterized in that only by varying the process parameters in the early stage of compression (temperature range 1400-1700 ° C), the Si 3 N 4 final structure is affected. 4. Das in den Ansprüchen 1-3 beschriebene Verfahren, dadurch gekennzeichnet, dass durch Variation der Aufheizrate während des Frühstadiums des Sinterprozesses (1400-1700°C) das Si3N4-Endgefüge beeinflußt wird. 4. The method described in claims 1-3, characterized in that the Si 3 N 4 final structure is influenced by varying the heating rate during the early stage of the sintering process (1400-1700 ° C). 5. Das in den Ansprüchen 1-4 beschriebene Verfahren, dadurch gekennzeichnet, dass durch Einfügen einer Haltezeit während des Frühstadiums des Sinterprozesses (1400-1700°C) das Si3N4-Endgefüge beeinflußt wird. 5. The method described in claims 1-4, characterized in that the Si 3 N 4 final structure is influenced by inserting a hold time during the early stage of the sintering process (1400-1700 ° C). 6. Das in den Ansprüchen 1-5 beschriebene Verfahren, dadurch gekennzeichnet, dass durch Erhöhung des N2-Gasdruckes während des Frühstadiums des Sinterprozesses (1400-1700°C) das Si3N4-Endgefüge beeinflußt wird. 6. The method described in claims 1-5, characterized in that the Si 3 N 4 final structure is influenced by increasing the N 2 gas pressure during the early stage of the sintering process (1400-1700 ° C). 7. Das in den Ansprüchen 1-6 beschriebene Verfahren, dadurch gekennzeichnet, dass durch Einfügen einer Haltezeit in Kombination mit der gleichzeitigen Erhöhung des N2-Gasdruckes während des Frühstadiums des Sinterprozesses (1400-1700°C) das Si3N4-Endgefüge beeinflußt wird. 7. The method described in claims 1-6, characterized in that by inserting a hold time in combination with the simultaneous increase in the N 2 gas pressure during the early stage of the sintering process (1400-1700 ° C) the Si 3 N 4 final structure being affected. 8. Das in den Ansprüchen 1-7 beschriebene Verfahren, dadurch gekennzeichnet, dass durch Absenkung der Temperatur während der Haltezeit in Kombination mit einer gleichzeitigen Erhöhung des N2-Gasdruckes während des Frühstadiums des Sinterprozesses (1400-1700°C) das Si3N4-Endgefüge beeinflußt wird. 8. The method described in claims 1-7, characterized in that by lowering the temperature during the holding time in combination with a simultaneous increase in the N 2 gas pressure during the early stage of the sintering process (1400-1700 ° C) the Si 3 N 4-end structure is affected. 9. Das in den Ansprüchen 1-8 beschriebene Verfahren, dadurch gekennzeichnet, dass das resultierende Si3N4-Endgefüge einen hohen Feinkornanteil und eine erhöhte Anzahl großer langgestreckter β-Si3N4-Körner, eingebettet in die feinkörnige Matrix, aufweist. 9. The method described in claims 1-8, characterized in that the resulting Si 3 N 4 final structure has a high proportion of fine grains and an increased number of large elongated β-Si 3 N 4 grains, embedded in the fine-grained matrix.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2266935A1 (en) * 2008-04-18 2010-12-29 Kabushiki Kaisha Toshiba Anti-wear member, anti-wear instrument and method of producing anti-wear member
EP3896300A4 (en) * 2018-12-11 2022-08-31 Kabushiki Kaisha Toshiba Sliding member, and bearing, motor and driving device using same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4113885A1 (en) * 1991-04-27 1992-10-29 Hoechst Ag METHOD FOR PRODUCING FINE-PARTICLE CRYSTALLINE SILICON NITRIDE
DE19629074A1 (en) * 1995-07-18 1997-01-23 Ngk Spark Plug Co High strength and hardness sintered silicon nitride-based material
DE19746283A1 (en) * 1996-10-25 1998-04-30 Electrolux Ab Suction line and cylinder inlet assembly for motorised saw

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4113885A1 (en) * 1991-04-27 1992-10-29 Hoechst Ag METHOD FOR PRODUCING FINE-PARTICLE CRYSTALLINE SILICON NITRIDE
DE19629074A1 (en) * 1995-07-18 1997-01-23 Ngk Spark Plug Co High strength and hardness sintered silicon nitride-based material
DE19746283A1 (en) * 1996-10-25 1998-04-30 Electrolux Ab Suction line and cylinder inlet assembly for motorised saw

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2266935A1 (en) * 2008-04-18 2010-12-29 Kabushiki Kaisha Toshiba Anti-wear member, anti-wear instrument and method of producing anti-wear member
EP2266935A4 (en) * 2008-04-18 2011-09-14 Toshiba Kk Anti-wear member, anti-wear instrument and method of producing anti-wear member
US8377837B2 (en) 2008-04-18 2013-02-19 Kabushiki Kaisha Toshiba Wear resistant member, wear resistant device and method for manufacturing the wear resistant member
EP3896300A4 (en) * 2018-12-11 2022-08-31 Kabushiki Kaisha Toshiba Sliding member, and bearing, motor and driving device using same

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