CN102701745B - Synthesis method of submicron claviform beta-Sialon - Google Patents
Synthesis method of submicron claviform beta-Sialon Download PDFInfo
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- CN102701745B CN102701745B CN201210164383.7A CN201210164383A CN102701745B CN 102701745 B CN102701745 B CN 102701745B CN 201210164383 A CN201210164383 A CN 201210164383A CN 102701745 B CN102701745 B CN 102701745B
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Abstract
The invention discloses a synthesis method of submicron claviform beta-Sialon, wherein silica sol, aluminum hydroxide, carbon black and ammonium chloride are used as raw materials, and then a right amount of Fe2O3 is added as catalyst; firstly, the raw materials are mixed, stirred and dried in order to prepare silicon-aluminum-carbon gel precursor with certain carbon-silicon ratio and silicon-aluminum ratio; then the precursor is subjected to the high-temperature reduction and nitridation in a certain nitrogen flow, so as to prepare the beta-Sialon powder. The reaction temperature is 1350 DEG C-1500 DEG C and the heat preservation time is 2-6h. The molecular formula of the obtained eta-Sialon is Si5AlON7; and according to the display of a scanning electron microscope, the synthetic beta-Sialon is claviform, about 0.4 mum in particle size, and about 98% in purity.
Description
One, technical field
The present invention relates to a kind of taking silicon gel as silicon source by carbothermic reduction-solgel reaction lesser temps preparation have higher degree, diameter is as the method for the bar-shaped beta-Sialon powder of submicron-scale.Belong to the field of chemical synthesis.
Two, background technology
Sialon material combines Si
3n
4excellent Physical and mechanical properties and Al
2o
3excellent chemical property., the feature such as thermal expansivity low, good in oxidation resistance high with its excellent hot strength, high rigidity, good heat-shock resistance, wear resistance, solidity to corrosion, toughness receives general concern.Be considered to one of most promising high-temperature structural material, all have a wide range of applications in fields such as metallurgy, automobile, oil, chemical industry, aerospace.
Preparation one of Sialon stupalith important channel be by after ceramic powder compression moulding again high temperature sintering become ceramic body, the main method of at present synthetic Sialon powder has by nitride and oxide high-temperature is synthetic or natural mineral is as synthetic in kaolin high temperature, the former is with high costs, the latter, due to the complicacy of natural matter composition, is difficult to obtain highly purified Sialon powder.Find economical, efficient and can scale production high quality the synthetic method of (purity is high, and fine size is uniformly dispersed good etc.) Sialon powder be a difficult problem urgently to be resolved hurrily.
Three, summary of the invention
The present invention aims to provide the synthetic method of the bar-shaped beta-Sialon of a kind of submicron, and technical problem to be solved is to reduce production costs in improving product purity.
In view of existing beta-Sialon powder preparation technology's current situation, new process should avoid using the problem of the ultra-fine nitride of high quality and the synthetic beta-Sialon powder somewhat expensive of oxide high-temperature, overcomes again and uses the synthetic not high puzzlement of beta-Sialon powder purity of natural mineral high temperature.
The present invention is taking silicon sol, aluminium hydroxide, carbon black and ammonium chloride as raw material, with Fe
2o
3for catalyzer, prepare and there is bar-shaped beta-Sialon powder higher degree, that diameter is submicron-scale by carbothermic reduction-sol-gel method reduction-nitridation.The molecular formula of gained beta-Sialon is Si
5alON
7.
Technical solution problem of the present invention adopts following technical scheme:
The synthetic method of the bar-shaped beta-Sialon of submicron of the present invention, comprises wet mixing, gel, dry, pyroreaction and the each unit process of thermal treatment:
Described wet mixing is to SiO
2massfraction is to add Al (OH) in 25% silicon sol
3, Fe
2o
3, carbon black and distilled water, within magnetic agitation 1-3 hour, obtain compound; Silica alumina ratio is 3-6:1, and carbon silicon mol ratio is 2-4:1, Fe
2o
3addition be SiO
2, Al (OH)
3, Fe
2o
30.5-3% with carbon black total mass;
Described gel is the ammonium chloride solution that adds mass concentration 25% in described compound, and add-on is gel with reaction solution and is as the criterion, and obtains presoma;
Described being dried is in 60-80 DEG C of dry 3-6 hour by presoma;
Described pyroreaction be by dried presoma in 1300-1500 DEG C of insulation reaction 2-6 hour, the flow with 1L/min in the process of reaction passes into nitrogen, obtains thick product;
Described thermal treatment de-carbon is that described thick product is obtained to the bar-shaped beta-Sialon powder of submicron in 600 DEG C of thermal treatment 3-6 hour.
The present invention is with silicon sol, aluminium hydroxide, carbon black, and ammonium chloride is raw material, prepares and has bar-shaped beta-Sialon powder higher degree, that diameter is submicron-scale.Raw material cheapness, preparation technology is simple, and less demanding, with low cost to equipment can and have the extensive synthetic new approach that provides of the beta-Sialon powder of better quality for economical and efficient.
Four, brief description of the drawings:
Fig. 1 is the XRD photo of the synthetic beta-Sialon powder of the present invention.As can be seen from Figure 1 product diffraction peak is mainly beta-Sialon diffraction peak, only has faint impurity peaks to exist, and illustrates that synthesized powder is single-phase beta-Sialon.
Fig. 2 is the SEM photo of the synthetic beta-Sialon powder of the present invention.As can be seen from Figure 2 the beta-Sialon powder of synthesized is bar-shaped, and particle diameter is 0.3-0.5 μ m.
Five, embodiment:
Embodiment 1:
Measure 20ml SiO
2massfraction is 25% silicon sol, is 5:1 by silica alumina ratio, and silicon-carbon mol ratio is that 3:1 weighs aluminium hydroxide and carbon black, Fe
2o
3addition be SiO
2, Al (OH)
3, Fe
2o
3with 2.5% of carbon black total mass, be placed in beaker and add 20ml distilled water magnetic stirrer 2 hours, slowly adding massfraction is 25% ammonium chloride solution, when add-on is about 10ml, mixture is transformed into gelinite and is presoma, presoma is dried to 6 hours in 60 DEG C, then in the electron tubes type High Temperature Furnaces Heating Apparatus that is 1L/min at nitrogen flow, 1400 DEG C are incubated 3 hours, finally within 5 hours, obtain beta-Sialon powder 600 DEG C of thermal treatments, and purity is 97%.
Embodiment 2:
Measure 20ml SiO
2massfraction is 25% silicon sol, is 5:1 by silica alumina ratio, and silicon-carbon mol ratio is that 3:1 weighs aluminium hydroxide and carbon black, Fe
2o
3addition be SiO
2, Al (OH)
3, Fe
2o
3with 1.0% of carbon black total mass, be placed in beaker and add 20ml distilled water magnetic stirrer 2 hours, slowly adding massfraction is 25% ammonium chloride solution, when add-on is about 10ml, mixture is transformed into gelinite and is presoma, presoma is dried to 3 hours in 80 DEG C, then in the electron tubes type High Temperature Furnaces Heating Apparatus that is 1L/min at nitrogen flow, 1450 DEG C are incubated 4 hours, finally within 6 hours, obtain beta-Sialon powder 600 DEG C of thermal treatments, and purity is 98%.
Embodiment 3:
Measure 20ml SiO
2massfraction is 25% silicon sol, is 5:1 by silica alumina ratio, and silicon-carbon mol ratio is that 3:1 weighs aluminium hydroxide and carbon black, Fe
2o
3addition be SiO
2, Al (OH)
3, Fe
2o
3with 0.5% of carbon black total mass, be placed in beaker and add 20ml distilled water magnetic stirrer 2 hours, slowly adding massfraction is 25% ammonium chloride solution, when add-on is about 10ml, mixture is transformed into gelinite and is presoma, presoma is dried to 5 hours in 70 DEG C, then in the electron tubes type High Temperature Furnaces Heating Apparatus that is 1L/min at nitrogen flow, 1500 DEG C are incubated 6 hours, finally within 6 hours, obtain beta-Sialon powder 600 DEG C of thermal treatments, and purity is 98.5%.
Claims (1)
1. a synthetic method for the bar-shaped beta-Sialon of submicron, comprises wet mixing, gel, dry, pyroreaction and the each unit process of thermal treatment, it is characterized in that:
Described wet mixing is to SiO
2massfraction is to add Al (OH) in 25% silicon sol
3, Fe
2o
3, carbon black and distilled water, within magnetic agitation 1-3 hour, obtain compound; Silica alumina ratio is 3-6:1, and carbon silicon mol ratio is 2-4:1, Fe
2o
3addition be SiO
2, Al (OH)
3, Fe
2o
30.5-3% with carbon black total mass;
Described gel is the ammonium chloride solution that adds mass concentration 25% in described compound, and add-on is gel with reaction solution and is as the criterion, and obtains presoma;
Described being dried is in 60-80 DEG C of dry 3-6 hour by presoma;
Described pyroreaction be by dried presoma in 1300-1500 DEG C of insulation reaction 2-6 hour, the flow with 1L/min in the process of reaction passes into nitrogen, obtains thick product;
Thermal treatment de-carbon is that described thick product is obtained to the bar-shaped beta-Sialon powder of submicron in 600 DEG C of thermal treatment 3-6 hour.
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| CN102061166A (en) * | 2011-01-07 | 2011-05-18 | 华东师范大学 | Method for synthesizing superfine ceramic fluorescent powder |
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| CN102061166A (en) * | 2011-01-07 | 2011-05-18 | 华东师范大学 | Method for synthesizing superfine ceramic fluorescent powder |
Non-Patent Citations (6)
| Title |
|---|
| Nano powders of β-sialon carbonthermal produced via a sol-gel process;Q.LI et al.;《JOURNAL OF MATERIALS SCIENCE LETTERS》;20031231;第22卷;第885－887页 * |
| Q.LI et al..Nano powders of β-sialon carbonthermal produced via a sol-gel process.《JOURNAL OF MATERIALS SCIENCE LETTERS》.2003,第22卷第885－887页. |
| 付芳.溶胶-凝胶和微波碳热还原氮化法合成β-sialon超细粉.《硅酸盐学报》.2007,第35卷(第3期),第317－321页. |
| 朱文振等.碳热还原法低温制备碳化硅微粉.《硅酸盐通报》.2012,第31卷(第1期),第46－49页. |
| 溶胶-凝胶和微波碳热还原氮化法合成β-sialon超细粉;付芳;《硅酸盐学报》;20070331;第35卷(第3期);第317-321页 * |
| 碳热还原法低温制备碳化硅微粉;朱文振等;《硅酸盐通报》;20120229;第31卷(第1期);第46－49页 * |
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