Mechanism and Kinetics of the Carbothermal Nitridation Synthesis of α-Silicon Nitride
The carbothermal nitridation synthesis of α‐Si3 N4is studied using electron microscopy techniques(FEG/SEM and TEM) and chemical composition analysis to characterize the reaction at various degrees of conversion. The reaction follows a nucleation‐growth mechanism. Without “seed”α‐Si3N4in the precurso...
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| Published in | Journal of the American Ceramic Society Vol. 80; no. 11; pp. 2853 - 2863 |
|---|---|
| Main Authors | , , , , |
| Format | Journal Article |
| Language | English |
| Published |
Westerville, Ohio
American Ceramics Society
01.11.1997
Blackwell Wiley Subscription Services, Inc |
| Subjects | |
| Online Access | Get full text |
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| Abstract | The carbothermal nitridation synthesis of α‐Si3 N4is studied using electron microscopy techniques(FEG/SEM and TEM) and chemical composition analysis to characterize the reaction at various degrees of conversion. The reaction follows a nucleation‐growth mechanism. Without “seed”α‐Si3N4in the precursor, the reaction rate is controlled by the formation of nuclei which are associated with a Si‐O‐C intermediate phase. In the presence of “seed,” the limiting step is growth of α‐Si3N4 onto the “seed” nuclei. Growth appears to follow a gas‐phase route and is characterized by an irregular porous layer which grows onto the “seed.” The porous structure is the result of reaction around car‐bon particles which are consumed during the process. The presence of admixed “seed” Si3N4in the precursor formu‐lation increases the reaction rate since the nucleation step is eliminated. An activation energy of E = 457 ± 55 kJ/mol for the overall reaction closely approximates that previously reported for the formation of SiO. This result, along with the finding that residual crystalline SiO2 is present at all stages of the reaction, indicates that the overall reactionrate is controlled by the reduction of SiO2. Since reaction at the carbon and SiO2 contact points is fast, the rate‐limiting step is most likely the gas‐phase carbon reduction of SiO2with CO. |
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| AbstractList | The carbothermal nitridation synthesis of alpha -Si sub 3 N sub 4 is studied using electron microscopy techniques (FEG/SEM and TEM) and chemical composition analysis to characterize the reaction at various degrees of conversion. The reaction follows a nucleation-growth mechanism. Without "seed" alpha -Si sub 3 N sub 4 in the precursor, the reaction rate is controlled by the formation of nuclei which are associated with a Si-O-C intermediate phase. In the presence of "seed", the limiting step is growth of alpha -Si sub 3 N sub 4 onto the "seed" nuclei. Growth appears to follow a gas-phase route and is characterized by an irregular porous layer which grows onto the "seed". The porous structure is the result of reaction around carbon particles which are consumed during the process. The presence of admixed "seed" Si sub 3 N sub 4 in the precursor formulation increases the reaction rate since the nucleation step is eliminated. An activation energy of E=457plus/minus55 kJ/mol for the overall reaction closely approximates that previously reported for the formation of SiO. This result, along with the finding that residual crystalline SiO sub 2 is present at all stages of the reaction, indicates that the overall reaction rate is controlled by the reduction of SiO sub 2 . Since reaction at the carbon and SiO sub 2 contact points is fast, the rate-limiting step is most likely the gas-phase carbon reduction of SiO sub 2 with CO. The carbothermal nitridation synthesis of alpha-Si3N4 is studied using electron microscopy techniques and chemical composition analysis to characterize the reaction at various degrees of conversion. The reaction follows a nucleation-growth mechanism. Without 'seed' alpha-Si3N4 in the precursor, the reaction rate is controlled by the formation of nuclei which are associated with a Si-O-C intermediate phase. In the presence of 'seed', the limiting step is growth of alpha-Si3N4 onto the 'seed' nuclei. Growth appears to follow a gas-phase route and is characterized by an irregular porous layer which grows onto the 'seed'. The porous structure is the result of reaction around carbon particles which are consumed during the process. The presence of admixed 'seed' Si3N4 in the precursor formulation increases the reaction rate since the nucleation step is eliminated. An activation energy of 457 +/- 55 kJ/mol for the overall reaction closely approximates that previously reported for the formation of SiO. This result, along with the finding that residual crystalline SiO2 is present at all stages of the reaction, indicates that the overall reaction rate is controlled by the reduction of SiO2. (Author) The carbothermal nitridation synthesis of α‐Si 3 N 4 is studied using electron microscopy techniques(FEG/SEM and TEM) and chemical composition analysis to characterize the reaction at various degrees of conversion. The reaction follows a nucleation‐growth mechanism. Without “seed”α‐Si 3 N 4 in the precursor, the reaction rate is controlled by the formation of nuclei which are associated with a Si‐O‐C intermediate phase. In the presence of “seed,” the limiting step is growth of α‐Si 3 N 4 onto the “seed” nuclei. Growth appears to follow a gas‐phase route and is characterized by an irregular porous layer which grows onto the “seed.” The porous structure is the result of reaction around car‐bon particles which are consumed during the process. The presence of admixed “seed” Si 3 N 4 in the precursor formu‐lation increases the reaction rate since the nucleation step is eliminated. An activation energy of E = 457 ± 55 kJ/mol for the overall reaction closely approximates that previously reported for the formation of SiO. This result, along with the finding that residual crystalline SiO 2 is present at all stages of the reaction, indicates that the overall reactionrate is controlled by the reduction of SiO 2 . Since reaction at the carbon and SiO 2 contact points is fast, the rate‐limiting step is most likely the gas‐phase carbon reduction of SiO 2 with CO. The carbothermal nitridation synthesis of α‐Si3 N4is studied using electron microscopy techniques(FEG/SEM and TEM) and chemical composition analysis to characterize the reaction at various degrees of conversion. The reaction follows a nucleation‐growth mechanism. Without “seed”α‐Si3N4in the precursor, the reaction rate is controlled by the formation of nuclei which are associated with a Si‐O‐C intermediate phase. In the presence of “seed,” the limiting step is growth of α‐Si3N4 onto the “seed” nuclei. Growth appears to follow a gas‐phase route and is characterized by an irregular porous layer which grows onto the “seed.” The porous structure is the result of reaction around car‐bon particles which are consumed during the process. The presence of admixed “seed” Si3N4in the precursor formu‐lation increases the reaction rate since the nucleation step is eliminated. An activation energy of E = 457 ± 55 kJ/mol for the overall reaction closely approximates that previously reported for the formation of SiO. This result, along with the finding that residual crystalline SiO2 is present at all stages of the reaction, indicates that the overall reactionrate is controlled by the reduction of SiO2. Since reaction at the carbon and SiO2 contact points is fast, the rate‐limiting step is most likely the gas‐phase carbon reduction of SiO2with CO. |
| Author | Weimer, Alan W. Beaman, Donald R. McCoy, Jeffrey W. Eisman, Glenn A. Susnitzky, David W. |
| Author_xml | – sequence: 1 givenname: Alan W. surname: Weimer fullname: Weimer, Alan W. organization: Ceramics and Advanced Materials Research, The Dow Chemical Company, Midland, Michigan 48667 – sequence: 2 givenname: Glenn A. surname: Eisman fullname: Eisman, Glenn A. organization: Ceramics and Advanced Materials Research, The Dow Chemical Company, Midland, Michigan 48667 – sequence: 3 givenname: David W. surname: Susnitzky fullname: Susnitzky, David W. organization: Ceramics and Advanced Materials Research, The Dow Chemical Company, Midland, Michigan 48667 – sequence: 4 givenname: Donald R. surname: Beaman fullname: Beaman, Donald R. organization: Ceramics and Advanced Materials Research, The Dow Chemical Company, Midland, Michigan 48667 – sequence: 5 givenname: Jeffrey W. surname: McCoy fullname: McCoy, Jeffrey W. organization: Ceramics and Advanced Materials Research, The Dow Chemical Company, Midland, Michigan 48667 |
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| Keywords | Carbothermy Chemical preparation Silicon Nitrides Reaction mechanism Nitriding Kinetics Experimental study Powder Non oxide ceramics Structural ceramic |
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| Notes | ark:/67375/WNG-GCCSR742-B istex:8161645E299F42A5650EDDDE261915074145614A ArticleID:JACE2853 Department of Chemical Engineering, University of Colorado, Boulder, Colorado 80309–0424. Manuscript No. 192018. Received February 15, 1996; approved April 7, 1997. Member, American Ceramic Society. Supported by the U.S. Department of Energy, Assistant Secretary for Energy Efficiency and Renewable Energy, Office of Transportation Technologies, as part of the Ceramic Technology Project of the Propulsion System Materials Program, under Contract No. DE–AC05–840R21400 with Martin Marietta Energy Systems, Inc. ObjectType-Article-2 SourceType-Scholarly Journals-1 ObjectType-Feature-1 content type line 23 |
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| Snippet | The carbothermal nitridation synthesis of α‐Si3 N4is studied using electron microscopy techniques(FEG/SEM and TEM) and chemical composition analysis to... The carbothermal nitridation synthesis of α‐Si 3 N 4 is studied using electron microscopy techniques(FEG/SEM and TEM) and chemical composition analysis to... The carbothermal nitridation synthesis of alpha-Si3N4 is studied using electron microscopy techniques and chemical composition analysis to characterize the... The carbothermal nitridation synthesis of alpha -Si sub 3 N sub 4 is studied using electron microscopy techniques (FEG/SEM and TEM) and chemical composition... |
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| SubjectTerms | Applied sciences Building materials. Ceramics. Glasses Ceramic industries Chemical industry and chemicals Exact sciences and technology Structural ceramics Technical ceramics |
| Title | Mechanism and Kinetics of the Carbothermal Nitridation Synthesis of α-Silicon Nitride |
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