CN100453508C - Chemically excited combustion process for synthesizing Si3N4/SiC composite powder - Google Patents
Chemically excited combustion process for synthesizing Si3N4/SiC composite powder Download PDFInfo
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- CN100453508C CN100453508C CNB2006100122517A CN200610012251A CN100453508C CN 100453508 C CN100453508 C CN 100453508C CN B2006100122517 A CNB2006100122517 A CN B2006100122517A CN 200610012251 A CN200610012251 A CN 200610012251A CN 100453508 C CN100453508 C CN 100453508C
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Abstract
The present invention belongs to the field of inorganic material technology, and is especially chemically excited combustion process for synthesizing Si3N4/SiC composite powder. The Si3N4/SiC composite powder is prepared with silica powder in 40-70 weight portions, carbon black in 20-50 weight portions, and chemical energizer in 0.5-20 weight portions, and through mg to obtain mixture, grinding and activating the mixture, loading in a high pressure reaction kettle in the bulk density of 0.3-1.0 g/cu cm, vacuum pumping and filling N2 or Ar in the pressure of 1-3 MPa, and inducing the mixture to produce self-spreading combustion synthesis reaction to prepare Si3N4/SiC composite powder. The process of the present invention has the advantages of simple steps, short production period, low power consumption and low cost.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, particularly a kind of chemical pumping burning synthesizing silicon nitride/silicon carbide (Si
3N
4/ SiC) the method for composite granule.
Background technology
Silicon nitride, silicon carbide ceramics are nearly 40 or the five ten years advanced high-temperature structural materials that grow up, and are typical case's representatives of non-oxide structure stupalith.They have good normal temperature and high-temperature behavior.Yet along with popularizing that stupalith is used, monophase materials exposes some shortcomings that can't overcome itself gradually, and is lower as fracture toughness property; The strength degradation that the sintering process grain growth causes etc. more and more cause people's attention so introduce the research of the nitride silicon based composite material of second phase in the silicon nitride ceramics matrix, and silicon carbide is a kind of that use at present is maximum, effect is best.Contain silicon nitride and silicon carbide biphase Si
3N
4/ SiC matrix material comprehensively has the advantage of silicon carbide high rigidity, silicon nitride high tenacity, has improved ceramic normal temperature and high-temperature behavior greatly, has improved ceramic stability, becomes the most rising stupalith.
Si
3N
4The preparation of/SiC matrix material mainly is divided into following several method: (1) is with Si
3N
4Mix back agglomerating method with two kinds of powder machineries of SiC; (2) reaction sintering; (3) carry out the agglomerating method with composite granule.The application just provides a kind of preparation Si
3N
4The method of/SiC composite granule is used for sintering high-performance Si
3N
4/ SiC matrix material.
At present, reported in literature prepares Si
3N
4The method of/SiC composite granule has gas-phase reaction method, carbothermal reduction-nitridation method, high-energy ball milling reaction method etc.The new former white first-class people of Japan prepares Si with gas-phase reaction
3N
4/ SiC composite granule, this composite granule mechanically mixes silicon nitride and silicon carbide powder further than simply, and the stupalith microstructure analysis for preparing with this composite granule shows this material Si
3N
4Crystal grain inside has the nano grade Sic particle, has constituted good nano SiC (the p)/Si of mechanical property
3N
4Matrix material.But its shortcoming is a desired raw material gas price costliness, the synthesis technique complexity, and equipment has high input, and preparation cost is very high.
The carbothermal reduction-nitridation method is the preparation Si that the research of Shanghai silicate institute is adopted
3N
4The method of/SiC composite granule.It is starting raw material that this method adopts home-made carbon black and aerogel silicon oxide, after the ball milling mixed number hour, puts into plumbago crucible, in High Temperature Furnaces Heating Apparatus, carries out carbothermic reduction reaction under the high pure nitrogen atmosphere, generates nanometer Si in 1500～1700 ℃ temperature range
3N
4/ SiC composite granule.The shortcoming of this method is, carbothermic reduction reaction energy consumption height, and the production cycle is long, and suitability for industrialized production is restricted.
People such as U.S. Shaw have studied with the synthetic Si of high-energy ball milling reaction method
3N
4/ SiC composite granule, this method are at NH with silica flour and graphite powder mix
3Or N
2Carry out high-energy ball milling in the atmosphere and handle,, both synthesized SiC/Si in the process of lapping through grinding for a long time
3N
4Composite granule.Yet this method only limits to the experimental study stage, also suitable distance will be arranged apart from suitability for industrialized production.
The combustion synthesis process that development in recent years is got up has advantages such as energy-conservation, efficient, low cost, the synthetic Si of burning
3N
4Powder has a large amount of research bases, and synthesizes SiC for burning, because the weak exothermal nature of reacting is difficult to directly prepare in the synthetic mode of burning, therefore adopts modes such as applying electric field, interpolation activator to promote to burn more and synthesizes the carrying out of SiC reaction.
Summary of the invention
The purpose of this invention is to provide a kind of chemical pumping burning synthesizing silicon nitride/silicon carbide (Si
3N
4/ SiC) the method for composite granule is in the technological process of synthesizing silicon nitride/silicon carbide composite powder body, by add chemical pumping agent NH in initial powder
4Cl and tetrafluoroethylene, the synthetic Si of burning in nitrogen atmosphere
3N
4/ SiC composite granule.
A further object of the present invention is simultaneously from the preparation technology of composite granule, and some processing parameter of appropriate change can prepare the powder that principal phase is SiC.
Chemical pumping burning synthesizing silicon nitride/silicon carbide (Si of the present invention
3N
4/ SiC) composite granule or principal phase are the method for SiC powder, this method may further comprise the steps:
(1) batching:
In weight part, with silica flour: 40～70 parts, carbon black: 20～50 parts, the chemical pumping agent: 0.5～20 part is mixed, and obtains a mixture;
Wherein said chemical pumping agent is NH
4Cl and tetrafluoroethylene, NH
4The weight ratio of Cl and tetrafluoroethylene is 1: 1～1: 10;
(2) activation treatment:
The mixture that step (1) is obtained grinds activation treatment;
(3) combustion reactions:
Mixture after step (2) ground is with 0.3～1.0g/cm
3Loose density pack in the autoclave, after vacuumizing, charge into nitrogen, make pressure-controlling at 1～3MPa, bring out mixture then and carry out the self-propagating combustion building-up reactions;
(4) reaction is finished:
After the rising of the elder generation of the pressure in the reactor slowly dropped to initial pressure again, combustion synthesis reaction was finished, the releasing reactor internal pressure, and resultant powdered product is Si
3N
4/ SiC composite granule.
The present invention has expanded the combustiblecomponents scope of raw material by changing content and the nitrogen equipressure that grinds activatory time, chemical pumping agent, has realized the synthetic Si of burning
3N
4/ SiC composite granule.Si/C/N
2Add chemical pumping agent NH in the reaction system
4Cl, its effect is the activating velocity that quickens the mechanical milling process material powder, makes reactant can realize particulate refinement and activation in the short period of time.Having added chemical pumping agent tetrafluoroethylene in the system, has been the effect of inducing combustion building-up reactions.
In the present invention, the particle size range of employed Si powder is 0.1～110 μ m; The particle size range of carbon black is 10～30nm; Employed chemical pumping agent is NH
4Cl and teflon mixture, wherein NH in the mixture
4The weight ratio of Cl and tetrafluoroethylene is 1: 1～1: 10.
In the blending process of step of the present invention (1), preferred earlier silica flour and carbon black being mixed in proportion adds chemical pumping agent NH then
4Cl carries out pre-activated and handles, and adds chemical pumping agent tetrafluoroethylene subsequently and carry out combination treatment (prevention chemical pumping agent tetrafluoroethylene is reunited) in process of lapping, also above chemical pumping agent can be added simultaneously and carry out mixing and ball milling.
Grind activation treatment for the mixture that step (1) is obtained, can adopt mechanical activation to handle, comprise that high-energy planetary formula ball milling, the horizontal rotor of high energy grind, high energy shakes grinding or stirring ball-milling etc., 1～10 hour ball milling time, preferred 1～5 hour.Then, the mix powder pine after grinding is loaded in the resistant to elevated temperatures container (for example porous graphite crucible), loose density is 0.3～1.0g/cm
3, put into reactor more together.The reactor that is used for the present invention is the high pressure vessel of the band watercooling jacket made with stainless steel.
In the present invention, adopt tungsten helix to make heating element, feed the electric current of 10～30A, bring out powder systems generation combustion synthesis reaction in the local heating mode.After the pressure fast rise in the reactor, illustrate that combustion synthesis reaction causes, the combustion synthesis reaction time is 10～30 minutes, the process that the pressure in the reactor slowly descends was both finished the process that is cooled to room temperature for reaction.Release reaction still internal pressure can obtain loose powdered product then, after the fine grinding, obtains Si
3N
4/ SiC composite granule.
From above preparation technology, to remove and change the nitrogen atmosphere in the reactor into pure argon atmosphere, the Si in the material powder, C blending ratio are suitably adjusted, and other reactive material and processing parameter are all with preparation Si
3N
4/ SiC composite granule can be prepared the powder that principal phase is SiC, no Si
3N
4Generate mutually.
The present invention compared with the prior art, its advantage is:
(1). the starting material powder is convenient can be got, and the raw material silica flour need not special processings such as pickling.
(2). the activation treatment time is only 1～10 hour ball milling time, preferred 1～5 hour; And combustion synthesis reaction is rapid, and whole combustion reaction time is 10～30 minutes, has shortened the whole production cycle.
(3). rely on the exothermic effect of raw material self to finish the self-propagating high-temperature reaction, after reaction is brought out, need not external energy, and the required electric energy of the chemical reaction that ignites can be ignored.Therefore, save energy reduces cost.
(4). owing to the introducing of chemical pumping agent and by grinding the equal activation treatment means of amorphous of introducing, realized being the direct ignition and the combustion synthesis reaction of weak thermopositive reaction agent system of principal phase with Si-C, and controlled reaction process effectively, make the synthetic required nitrogen pressure of burning reduce (reaction pressure 1～3MPa).And then reduced requirement to equipment, improved the production safety coefficient.
(5). the present invention can also prepare Si respectively by the adjustment to processing parameter and proportioning raw materials
3N
4/ SiC composite granule or principal phase are the powder of SiC, have realized the widespread use of this technology in low heat release combustion system.
Description of drawings
Fig. 1. the XRD spectra of the β-SiC powder of preparation in the embodiment of the invention 3.
Fig. 2. the β-SiC powder SEM photo of preparation in the embodiment of the invention 3.
Embodiment
Embodiment 1
Si powder, the carbon black of median size 30nm, the NH of median size 0.5 μ m
4Cl and tetrafluoroethylene, by weight than 60: 30: 5: 5 take a sample, and they are put into the ball grinder ball milling 9 hours of vibromill, make its thorough mixing and activation; Material behind the admixture activation is placed the porous graphite crucible, make loose density be about 0.3～1.0g/cm
3, place a helically wound tungsten filament on the material upper strata, the tungsten filament diameter is 0.5mm, puts into the combustion synthesis reaction still more together; After vacuumizing, charge into high pure nitrogen, reach 2MPa up to nitrogen pressure from the reactor bottom; Helical tungsten filament is passed to the pulsed current of 10～30A, make its heating, bring out the material powder self-propagating combustion, combustion reactions continues to be cooled to room temperature after 10 minutes, reaction end gas is emitted again, and the fine grinding product promptly obtains combustion reaction products.Reaction product is carried out material phase analysis with Japan's D/MAX-IIB type X-ray diffraction analyser of science, and its result is Si
3N
4/ SiC composite granule.
Embodiment 2
Si powder, the carbon black of median size 20nm, the NH of median size 5 μ m
4Cl and tetrafluoroethylene, by weight than 70: 25: 2: 3 take a sample, will claim earlier Si powder, carbon black and NH
4Cl puts into the ball grinder ball milling 5 hours of planetary ball mill, makes its thorough mixing, tetrafluoroethylene is added again, and continues milled processed 1 hour; Mixed material is placed in the porous graphite crucible, make loose density be about 0.3～1.0g/cm
3, place a helical tungsten filament on the material upper strata, put into the combustion synthesis reaction still more together; After vacuumizing, charge into nitrogen to 1MPa from the reactor bottom; Helical tungsten filament is passed to the pulsed current of 12A, make its heating, bring out the material powder self-propagating combustion, combustion reactions continues to be cooled to room temperature after 30 minutes, emptying gas, and the fine grinding product promptly obtains reaction product.Reaction product is carried out material phase analysis with Japan's D/MAX-IIB type X-ray diffraction analyser of science, and with HITACHI S-4300 scanning electron microscopic observation products of combustion pattern, test result proves that combustion synthesized product is Si
3N
4/ SiC composite granule.
Embodiment 3
Si powder, the carbon black of median size 10nm, the NH of median size 44 μ m
4Cl and tetrafluoroethylene, by weight than 52: 31: 2: 15 take a sample, and put into the ball grinder of oscillatory type ball mill, and ball milling 4.5 hours makes its thorough mixing and activation; Material behind the admixture activation is placed the porous graphite crucible, make loose density be about 0.3～1.0g/cm
3, place a helically wound tungsten filament on the material upper strata, the tungsten filament diameter is 0.5mm, puts into the combustion synthesis reaction still more together; After vacuumizing, charge into argon gas to 3MPa from the reactor bottom; Helical tungsten filament is passed to the pulsed current of 12A, make its heating, bring out the material powder self-propagating combustion, combustion reactions continues to be cooled to room temperature after 15 minutes, emptying gas, the fine grinding product, get final product reaction product.Reaction product is carried out XRD analysis with Japan's D/MAX-IIB type X-ray diffraction analyser of science, and with HITACHI S-4300 scanning electron microscopic observation products of combustion pattern, the test result demonstration, combustion synthesized product is pure β-SiC powder, no Si
3N
4Exist mutually.The XRD spectra of this powder and SEM photo are seen Fig. 1 and Fig. 2.
Claims (10)
1. the method for chemical pumping burning synthesizing silicon nitride/silicon carbide composite powder body is characterized in that this method may further comprise the steps:
(1) batching:
In weight part, with silica flour: 40～70 parts, carbon black: 20～50 parts, the chemical pumping agent: 0.5～20 part is mixed, and obtains a mixture;
Wherein said chemical pumping agent is NH
4Cl and tetrafluoroethylene, NH
4The weight ratio of Cl and tetrafluoroethylene is 1: 1～1: 10;
(2) activation treatment:
The mixture that step (1) is obtained grinds activation treatment;
(3) combustion reactions:
Mixture after step (2) ground is with 0.3～1.0g/cm
3Loose density pack in the autoclave, after vacuumizing, charge into nitrogen, make pressure-controlling at 1～3MPa, bring out mixture then and carry out the self-propagating combustion building-up reactions;
(4) reaction is finished:
After the rising of the elder generation of the pressure in the reactor slowly dropped to initial pressure again, combustion synthesis reaction was finished, the releasing reactor internal pressure, and resultant powdered product is Si
3N
4/ SiC composite granule.
2. the synthetic principal phase of chemical pumping burning is the method for the powder of SiC, it is characterized in that this method may further comprise the steps:
(1) batching:
In weight part, with silica flour: 40～70 parts, carbon black: 20～50 parts, the chemical pumping agent: 0.5～20 part is mixed, and obtains a mixture;
Wherein said chemical pumping agent is NH
4Cl and tetrafluoroethylene, NH
4The weight ratio of Cl and tetrafluoroethylene is 1: 1～1: 10;
(2) activation treatment:
The mixture that step (1) is obtained grinds activation treatment;
(3) combustion reactions:
Mixture after step (2) ground is with 0.3～1.0g/cm
3Loose density pack in the autoclave, after vacuumizing, charge into argon gas, make pressure-controlling at 1～3MPa, bring out mixture then and carry out the self-propagating combustion building-up reactions;
(4) reaction is finished:
After the rising of the elder generation of the pressure in the reactor slowly dropped to initial pressure again, combustion synthesis reaction was finished, and releasing reactor internal pressure, resultant powdered product are that principal phase is the powder of SiC.
3. method according to claim 1 and 2 is characterized in that: the blending process of described step (1) is earlier silica flour and carbon black to be mixed in proportion, and adds chemical pumping agent NH then
4Cl carries out pre-activated and handles, and adds chemical pumping agent tetrafluoroethylene subsequently and carries out combination treatment.
4. method according to claim 1 and 2 is characterized in that: the particle size range of described silica flour is 0.1～110 μ m; The particle size range of described carbon black is 10～30nm.
5. method according to claim 3 is characterized in that: the particle size range of described silica flour is 0.1～110 μ m; The particle size range of described carbon black is 10～30nm.
6. method according to claim 1 and 2 is characterized in that: the described grinding activation treatment time is 1～10 hour.
7. method according to claim 6 is characterized in that: described grinding activation treatment adopts mechanical activation to handle, and grinds activation treatment machinery and comprises that high-energy planetary formula ball milling, the horizontal rotor of high energy grind, the high energy vibrations are ground or stirring ball-milling.
8. method according to claim 1 and 2 is characterized in that: described mixture after step (2) is ground is packed in the reactor, is that the mix powder pine after will grinding earlier is loaded in the resistant to elevated temperatures porous graphite crucible, and then puts into reactor together.
9. method according to claim 1 and 2, it is characterized in that: describedly bring out mixture to carry out combustion synthesis reaction be to adopt tungsten helix to make heating element, feed the electric current of 10～30A, bring out mixture in the local heating mode and carry out the self-propagating combustion building-up reactions.
10. method according to claim 9 is characterized in that, the described combustion synthesis reaction time is 10～30 minutes.
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| CN102161587B (en) * | 2011-03-28 | 2013-06-19 | 北京理工大学 | Method for preparing transitional metal-doped silicon carbide material through self-propagation high-temperature synthesis |
| CN103641484A (en) * | 2013-12-16 | 2014-03-19 | 武汉科技大学 | Method for preparing Si3N4/SiC composite ceramic powder from biomass power plant ash |
| CN104150911B (en) * | 2014-07-14 | 2016-07-06 | 安徽理工大学 | A kind of method of microwave-assisted quickly synthesis in low temperature nano-silicon nitride-silicon carbide composite powder body |
| CN104496485B (en) * | 2014-12-08 | 2016-06-08 | 武汉科技大学 | The preparation method of a kind of silicon nitride or silicon nitride/silicon carbide composite granule |
| CN104878239A (en) * | 2015-06-15 | 2015-09-02 | 白城福佳科技有限公司 | High-temperature self-propagating synthesis method of silicon-manganese nitride alloy |
| CN105503198B (en) * | 2015-11-30 | 2017-10-17 | 衡阳凯新特种材料科技有限公司 | Silicon nitride material and preparation method thereof |
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| CN105884373B (en) * | 2016-04-18 | 2018-08-24 | 西峡县新越冶金材料开发有限公司 | A method of preparing silicon nitride |
| CN109530715B (en) * | 2018-12-13 | 2021-12-14 | 西安工程大学 | Preparation method of nickel nano powder for ceramic capacitor |
| CN109650903A (en) * | 2019-01-14 | 2019-04-19 | 江苏大学 | A kind of carbon solid solution nitriding silicon materials and preparation method thereof |
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| WO2000032537A2 (en) * | 1998-12-03 | 2000-06-08 | Cfi Ceramics For Industry Gmbh & Co. Kg | Reaction-bonded silicon nitride-based materials and method for producing the same |
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2006
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|---|---|---|---|---|
| WO2000032537A2 (en) * | 1998-12-03 | 2000-06-08 | Cfi Ceramics For Industry Gmbh & Co. Kg | Reaction-bonded silicon nitride-based materials and method for producing the same |
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Assignee: Zibo Luzhong Refractory Co., Ltd. Assignor: Technical Institute of Physics and Chemistry, CAS Contract fulfillment period: 2009.9.15 to 2016.9.14 Contract record no.: 2009370000302 Denomination of invention: Chemically excited combustion process for synthesizing Si3N4/SiC composite powder Granted publication date: 20090121 License type: Exclusive license Record date: 20090921 |
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