CN101786165B - Method for synthesizing Nb/Nb5Si3 composite materials at high temperature through microwave induced self propagating - Google Patents

Method for synthesizing Nb/Nb5Si3 composite materials at high temperature through microwave induced self propagating Download PDF

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CN101786165B
CN101786165B CN2009102734899A CN200910273489A CN101786165B CN 101786165 B CN101786165 B CN 101786165B CN 2009102734899 A CN2009102734899 A CN 2009102734899A CN 200910273489 A CN200910273489 A CN 200910273489A CN 101786165 B CN101786165 B CN 101786165B
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sintering
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CN101786165A (en
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王爱华
杨妮
闫华
宋武林
董选普
李建军
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Abstract

The invention provides a method for synthesizing Nb/Nb5Si3 composite materials at a high temperature through microwave induced self propagating, which consists of an ingredient recipe and a synthesis technology, wherein the ingredient recipe comprises pure niobium powder and pure silicon powder according to a mixing ratio of Nb-(5-37.5 at.%)Si, and the synthesis technology comprises the following steps: (1), firstly, proportionally and uniformly mixing all ingredient powder in the ingredient recipe to obtain composite powder; (2) grinding the composite powder into fine powder with the granularity of 800 meshes; (3) forming the ground composite powder at the pressure between 100 and 300 MPa; and (4) placing the formed materials into a microwave cavity for self propagating sintering by the microwaves under the protection of argon gas, and flowing argon gas is inflated into the microwave cavity during the self propagating sintering after vacuum pumping. The invention fully utilizes the advantages of the microwave sintering technology and the self propagating high-temperature synthesis, synthesized test samples do not contain oxide, the preparation time is short, and the reaction is complete.

Description

A kind of microwave induced self propagating high temperature synthesizes Nb/Nb＜sub〉5＜/sub〉Si＜sub〉3＜/sub〉method of composite
Technical field
The present invention relates to microwave technology and high-temperature structural material technology, a kind of specifically microwave induced self propagating high temperature synthesizes Nb/Nb 5Si 3The method of composite.A kind of original position is synthesized Nb/Nb 5Si 3The new method of high temperature structural composite material.
Background technology
Transition metal silicide is owing to have high-melting-point, low-density and thermal conductivity, and especially the high-temperature behavior of excellence under the condition of high temperature has been subjected to common concern both domestic and external.The silicide of using as structure is mainly by producing in Mo-Si, Nb-Si and the Ti-Si system.Nb 5Si 3The fusing point of (2480 ℃) is higher, the lower (7.16g/cm of density 3).And this compound also has good antioxygenic property and electric conductivity.Therefore, potential application prospect is arranged on high-temperature structural material.Though Nb 5Si 3Potential application prospect is arranged on high-temperature structural material.But, as other intermetallic compound, Nb 5Si 3Toughness at room temperature and cold and hot working ability are relatively poor, thereby have hindered its application in high-temperature structural material.In order to overcome low this defective of silicide toughness, can in silicide, introduce the metal phase.Result of study shows that the in-situ composite toughness of this intermetallic compound and metal second phase composition is fine, and that wherein prominent is Nb/Nb 5Si 3In-situ composite, its fracture toughness up to
Figure G2009102734899D00011
Tissue is stable when 1500 ℃ of long-term insulations.
The Nb based high-temperature alloy is generally by niobium solid solution Nbss and Nb 3Si, Nb 5Si 3Or the equal metal of Laves is asked the compound composition.The non-oxidizability of discovering Nbss is poor, and silicide is low with Laves room temperature fracture toughness mutually, and these shortcomings have hindered the application of Nb based high-temperature alloy.Alloying is a kind of material creep resistance, non-oxidizability simply and effectively improved, and obtains the approach of room temperature and high-temperature comprehensive property.The interpolation of alloying element and the difference of constituent content all can cause Nb based high-temperature alloy microstructure, and as the variation of primary phase, eutectic structure pattern, and this variation will finally cause the difference of material mechanical performance.The main alloy element of Nb based high-temperature alloy has Ti, Mo, and Cr, Hf, Al, B etc., for example: the interpolation of Cr, Al, W, Mo, V, Zr and Re becomes fragile Nb, has improved its crisp ductility transition temperature (BDTT); The interpolation of Ti and Hf has then reduced the crisp ductility transition temperature of Nb, but the interpolation of Cr and Al significantly improves the antioxygenic property of alloy; Interpolation Mo can improve the fusing point and the elevated temperature strength of niobium silicide base alloy, suppresses eutectic reaction L → Nbss+Nb 3The generation of Si, and impel Nbss+ β-(Nb, Mo) 5Si 3Eutectic reaction take place, Mo also has significant solution strengthening effect to niobium silicide base alloy; The adding of Fe makes niobium-silicon alloy have superplasticity more than 1350 ℃, and its tensile elongation can reach 512% in the time of 1450 ℃.
Synthetic being meant of microwave burning utilizes microwave irradiation to replace traditional thermal source, and mixed uniformly material reaches certain high temperature by self to the absorption (or dissipation) of microwave energy, thereby causes the building-up process of burning.As everyone knows, in microwave heating process, the distribution in temperature field is opposite with normal conditions, for example, the temperature height of idiosome temperature inside specific surface, this is because in microwave heating process, heat scatters and disappears to external environment condition from idiosome inside.Therefore, in the combustion reaction that microwave ignites, light earlier the inside of idiosome, and combustion wave is outwards propagated very fast again then.This just makes that the form of the product that heating using microwave and traditional external heat are prepared is completely different, and the conversion of the reactant that also makes is more thorough, and promptly reaction is more complete.Thereby the microwave self-propagating reaction that ignites is a frontier that causes extensive concern.But in recent years, heating using microwave only under lab apply to the synthetic or self propagating high temperature of reaction synthetic on.In order to make the microwave self-propagating reaction that successfully ignites, the dielectric properties of precursor are the factors of most critical.The reactant of suitable microwave assistant self propagating high temperature synthetic reaction must absorb microwave energy, thereby reactant can be heated to higher temperature within a short period of time, to produce the reaction of igniting and self propagating high temperature.Nineteen ninety, the Dalton of Univ Florida USA etc. takes the lead in proposing the application of heating using microwave in self propagating high temperature is synthetic.Through the development in 20 years nearly, especially after 2000, carry out extensive studies abroad, but domestic less about the synthetic concern of microwave induced burning to microwave induced burning is synthetic, it is synthetic to be that Shanghai silicate research institute is applied to the Sialon pottery the earliest.Though have other scientific research institution that other material system is studied at present, all also do not go deep into, concrete research yet.Experiment showed, under suitable condition of the synthetic aspect of microwave auxiliary combustion, the sparking mode of igniting in inside radially spreads at its burning beacon of most applications.When closing microwave source, spreading of beacon of burning stops, and this means the propagation that perhaps can control the burning beacon by the switch of microwave source, and can obtain the performance more excellent than traditional heating by the synthetic material of microwave induced burning aspect a lot.At present, though the microwave auxiliary combustion is synthetic to be widely used in the synthetic of a lot of material systems, the synthetic article that is applied to transition metal silicide is very few, and has all obtained to be better than the performance of normal sintering.For example, the combustion product reaction is more complete.At synthetic CoSi 2Combustion reaction in, the component synthetic by microwave pilot combustion synthetic method is CoSi entirely 2Phase, and the synthetic component of conventional burning contains CoSi 2With Si mutually.Synthetic CoSi and the CoSi of containing of thermal excitation burning 2Phase.Equally at Mo 5Si 3Synthetic in, have only the synthetic product of microwave induced burning only to contain Mo and Mo 5Si 3Phase does not contain other accessory substance.
Vacuum arc melting is preparation Nb/Nb 5Si 3The common method of composite, this method is to Nb/Nb 5Si 3Positive impetus has been played in the development of composite and application.Yet this method remained in energy consumption height (remelting more than three times), cycle long (only heat treatment time is just up to 100h), and operation many (founding+hot extrusions) etc. are not enough.Therefore, be necessary exploitation preparation Nb/Nb 5Si 3The new technology of composite.
At present, about preparation Nb/Nb 5Si 3The patent of composite aspect also seldom, patent " a kind of niobium-titanium-silicon-zirconium-hafnium-boron alloy and preparation method thereof " (patent publication No. 101235455) forms High-Temperature Strengthening phase Nb by adding element silicon to impel in the alloy in niobium-base alloy 5Si 3, Nb 5Si 3Formation can improve the room temperature toughness of niobium-base alloy and make alloy keep the certain high temperature mechanical property.And patent " a kind of iridium niobium silicon high temperature alloy material and preparation method thereof " (patent publication No. 1786236) and patent " the chromium modified silicide coating of resistance to high temperature oxidation and the preparation method of coating thereof " (patent publication No. 1818124) also all only relate to niobium silicon and other element forms high-temperature material together, not the formation of Nb5Si3.
Summary of the invention
The object of the present invention is to provide a kind of microwave induced self propagating high temperature to synthesize Nb/Nb 5Si 3The method of composite makes it can be in the short time, the synthetic Nb/Nb of original position under the lower energy consumption 5Si 3Composite.
For achieving the above object, the present invention adopts following technical scheme: a kind of microwave induced self propagating high temperature synthesizes Nb/Nb 5Si 3The method of composite, this method is made up of composition of raw materials and synthesis technique, and described composition of raw materials comprises pure niobium powder and pure silicon powder, and its proportioning is Nb-(5-37.5at.%) Si, and described synthesis technique comprises the steps:
(1) batching: at first each material powder in the composition of raw materials is mixed in proportion into composite powder;
(2) grind: it is 800 purpose fine powders that above-mentioned composite powder is ground to form granularity;
(3) moulding: make composite powder after the above-mentioned grinding at the forming under the pressure of 100-300MPa;
(4) spread sintering certainly: molded material is put into microwave cavity and is carried out charging into mobile argon gas after vacuumizing in the microwave cavity when spreading sintering certainly from spreading sintering with microwave under argon shield.
After spreading sintering and finishing, close microwave source, sample is taken out in the cold back of stove.
In such scheme, described composition of raw materials can also comprise: any one among B, C, Al, Fe, Hf, W, Mo, V, Ti and the Cr or two or more multiple alloy powders, any consumption is the 1-5at% of total raw material consumption in the alloy powder of above-mentioned B, C, Al, Fe and Hf, any consumption is the 5-15at% of total raw material consumption among W, Mo, V, Ti and the Cr, then each material powder in the composition of raw materials is mixed in proportion the polynary composite powder of preparation.
Spreading certainly in the sintering circuit in such scheme, heating rate is preferably 10-100 ℃/min, spreads the preferred 1200-1500 of sintering temperature ℃ certainly, and temperature retention time is no more than 30min.
Certainly spread in the temperature-rise period of sintering circuit above-mentioned, the low thermophase below 350 degree, heating rate is preferably 10-40 ℃/min, and at the above hot stage of 350 degree, heating rate is preferably 40-100 ℃/min to spreading sintering temperature certainly.
Spreading certainly in the sintering circuit in such scheme can be imbedded Al with the sample after the moulding 2O 3, put into microwave cavity behind the protection powder that mixes of SiC and Al and carry out from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 18wt%, SiC:80wt%, Al:2wt%.
Spreading certainly in the sintering circuit in such scheme also can be imbedded Al with the sample after the moulding 2O 3, put into microwave cavity behind the protection powder that mixes of SiC and C and carry out from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 20wt%, SiC:78wt%, C:2wt%.
Spreading certainly in the sintering circuit in such scheme preferably is evacuated to below the 2Pa in the microwave cavity.
In the grinding step in such scheme, can adopt planetary ball mill to composite powder ball milling 2-48h, ball-milling medium is an alcohol, ball material weight ratio 3: 1, and the stearic acid of adding 2wt% is as process control agent.
The present invention is spreading in the sintering circuit certainly, utilizes between microwave induced Nb, the Si self-propagating reaction takes place, and in building-up process, the self-propagating reaction extreme temperatures can evaporate volatile impurity, thereby power consumption is few, the product purity height.Consider microwave sintering densification rate height, sintering temperature is high more, and sintering time is long more, and sintered body is fine and close more, but crystal grain also can be grown up along with the growth of sintering temperature and sintering time simultaneously, destroys the performance of material.And high temperature rapid firing and low temperature burns slowly all can cause and organizes crystallite dimension inhomogeneous, phenomenon such as pore-size is excessive.Therefore, at the following low thermophase of 350 degree, that heating rate is selected is slow (10-40 ℃/min) with the binding agent in the removal sample.Be rapidly heated more than 350 degree (40-100 ℃/min) to sintering temperature.So whole heating rate is controlled to be 10-100 ℃/min in the sintering process from spreading, sintering temperature 1200-1500 ℃, temperature retention time is no more than 30min.
The present invention from spreading in the sintering circuit, imbeds Al with the sample after the moulding described 2O 3, put into microwave cavity behind the protection powder that mixes of SiC and Al and carry out from spreading sintering.SiC is a kind of powder that is easy to inhale ripple, uses the SiC powder can effectively prevent the sample cracking that causes owing to problems such as the too high thermograde that produces on the material diverse location, thermal runaways as the auxilliary hot material of microwave.But it is low or too high that SiC powder concentration is crossed, with regard to deficiency so that the temperature of microwave sintering reaches sintering Nb/Nb 5Si 3Therefore the temperature that composite is required needs certain Al 2O 3The concentration of powder dilute Si C powder.So the proportioning of above-mentioned protection powder is Al 2O 3: 18wt%, SiC:80wt%, Al:2wt%.
Equally, the sample after the moulding is imbedded Al 2O 3, put into microwave cavity behind the protection powder that mixes of SiC and C and carry out from spreading sintering, with aforementioned the same, ftracture in order to prevent sample, and make the microwave sintering temperature reach Nb/Nb 5Si 3The sintering temperature that composite is required, the proportioning of above-mentioned protection powder are Al 2O 3: 20wt%, SiC:78wt%, C:2wt%.
Characteristics of the present invention: under the Nb-Si material system, by heating using microwave with spread combination process certainly and prepared Nb-Nb 5Si 3Composite; Especially spreading certainly in the sintering process, adopting Al 2O 3+ SiC+C and Al 2O 3Two kinds of material systems of+SiC+Al are imbedded protection, only are under the situation of 2Pa, to have avoided the oxidation reaction of material fully in vacuum, have synthesized highly purified Nb-Nb 5Si 3Composite.
Description of drawings
Fig. 1 is the XRD figure spectrum that the Nb-37.5at%Si sample vacuumizes the back direct sintering among the embodiment 1;
Fig. 2 is that the Nb-18.7at%Si sample is imbedded Al among the embodiment 2 2O 3XRD figure spectrum in the+SiC+C powder behind the sintering;
Fig. 3 is that the Nb-18.7at%Si sample buries Al among the embodiment 3 2O 3XRD figure spectrum in the+SiC+Al powder behind the sintering;
Fig. 4 is that the Nb-5at%Si sample is imbedded Al among the embodiment 4 2O 3XRD figure spectrum in the+SiC+C powder behind the sintering;
Fig. 5 is that the Nb-18Si-2Al sample is imbedded Al among the embodiment 5 2O 3XRD figure spectrum in the+SiC+C powder behind the sintering;
Fig. 6 is that Nb-Si-Mo system sample is imbedded Al among the embodiment 6 2O 3XRD figure spectrum in the+SiC+Al powder behind the sintering
Fig. 7 Nb-14Ti-18Si-10Cr-5Al-10Mo sample is imbedded Al 2O 3XRD figure spectrum in the+SiC+C powder behind the sintering
The specific embodiment
Embodiment 1:
So far carry out under argon shield after the Nb-37.5at%Si sample vacuumizes from spreading sintering with Nb, the Si powder is pressed Nb 5Si 3Chemical formula preparation Nb: the Si atomic ratio is 62.5: 37.5 a composite powder, and ball milling 10h in planetary ball mill, ball-milling medium are alcohol, and ratio of grinding media to material is 3: 1, and the stearic acid that adds 2wt% is as process control agent.Behind the sample drying behind the ball milling at the forming under the pressure of 300MPa.Sample after the moulding is put into microwave cavity, is evacuated to charge into mobile argon gas behind the 2Pa, carries out under argon shield from spreading sintering.Start microwave source, heating rate is 10-40 ℃/min, 1200 ℃ of sintering temperatures, temperature retention time 15min.Sample is taken out in the cold back of stove.Sample after burning till is mainly by the oxide of niobium, SiO 2And minor N b 3Si and Nb 5Si 3Form.Its XRD figure spectrum is shown as Fig. 1.This explanation can prepare Nb preferably under this material composition and experiment condition 5Si 3, but have certain oxidative phenomena.
Embodiment 2:
The Nb-18.7at%Si sample is imbedded Al 2O 3Carry out in+SiC+C the powder from spreading sintering
With Nb, the Si powder is prepared Nb by eutectic composition: the Si atomic ratio is 81.3: 18.7 a composite powder, and ball milling 10h in planetary ball mill, ball-milling medium are alcohol, and ratio of grinding media to material is 3: 1, and the stearic acid of adding 2wt% is as process control agent.Behind the sample drying behind the ball milling at the forming under the pressure of 100MPa.Sample after the moulding is imbedded Al 2O 3Put into microwave cavity after in+SiC+C the powder, be evacuated to and charge into mobile argon gas behind the 2Pa, carry out under argon shield from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 20wt%, SiC:78wt%, C:2wt%.Start microwave source, heating rate is 10-40 ℃/min, 1300 ℃ of sintering temperatures, temperature retention time 30min.Sample is taken out in the cold back of stove.Sample after burning till is mainly by Nb, Nb 5Si 3And minor N b 3Si, NbC forms.Its XRD figure spectrum is shown as Fig. 2.This explanation is by imbedding Al 2O 3Carry out sintering in the+SiC+C powder, avoided the oxidation of powder fully, synthetic Nb 5Si 3Purity higher.
Embodiment 3:
The Nb-18.7at%Si sample is imbedded Al 2O 3Carry out in+SiC+Al the powder from spreading sintering
With Nb, the Si powder is prepared Nb by eutectic composition: the Si atomic ratio is 81.3: 18.7 a composite powder, and ball milling 10h in planetary ball mill, ball-milling medium are alcohol, and ratio of grinding media to material is 3: 1, and the stearic acid of adding 2wt% is as process control agent.Behind the sample drying behind the ball milling at the forming under the pressure of 300MPa.Sample after the moulding is imbedded Al 2O 3Put into microwave cavity after in+SiC+Al the powder, be evacuated to and charge into mobile argon gas behind the 2Pa, carry out under argon shield from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 18wt%, SiC:80wt%, Al:2wt%.Start microwave source, heating rate is 10-40 ℃/min, 1300 ℃ of sintering temperatures, temperature retention time 30min.Sample is taken out in the cold back of stove.Sample after burning till is mainly by Nb, Nb 5Si 3And minor N b 3Si forms.Its XRD figure spectrum as shown in Figure 3.
Embodiment 4:
Nb-5at%Si imbeds Al 2O 3Carry out in+SiC+C the powder from spreading sintering
With Nb, the Si powder is mixed with Nb: the Si atomic ratio is 95: 5 a composite powder, and ball milling 10h in planetary ball mill, ball-milling medium are alcohol, and ratio of grinding media to material is 3: 1, and the stearic acid of adding 2wt% is as process control agent.Behind the sample drying behind the ball milling at the forming under the pressure of 300MPa.Sample after the moulding is imbedded Al 2O 3Put into microwave cavity after in+SiC+C the powder, be evacuated to and charge into mobile argon gas behind the 2Pa, carry out under argon shield from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 20wt%, SiC:78wt%, C:2wt%.Start microwave source, heating rate is 10-40 ℃/min, 1400 ℃ of sintering temperatures, temperature retention time 30min.Sample is taken out in the cold back of stove.Sample after burning till is mainly by Nb, Nb 5Si 3And minor N b 3Si forms.Its XRD figure spectrum as shown in Figure 4.
Embodiment 5:
Nb-18Si-2Al imbeds Al 2O 3Carry out in+SiC+C the powder from spreading sintering
With Nb, Si, the Al powder is mixed with Nb: Si: the Al atomic ratio is 80: 18: 2 a composite powder, and ball milling 10h in planetary ball mill, ball-milling medium are alcohol, and ratio of grinding media to material is 3: 1, and the stearic acid of adding 2wt% is as process control agent.Behind the sample drying behind the ball milling at the forming under the pressure of 300MPa.Sample after the moulding is imbedded Al 2O 3Put into microwave cavity after in+SiC+C the powder, be evacuated to and charge into mobile argon gas behind the 2Pa, carry out under argon shield from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 20wt%, SiC:78wt%, C:2wt%.Start microwave source, heating rate is 10-40 ℃/min, 1400 ℃ of sintering temperatures, 1480 ℃.Temperature retention time 30min.Sample is taken out in the cold back of stove.1400 ℃ of samples after burning till are mainly by Nb, Nb 5Si 3And minor N b 3Si forms.1480 ℃ of samples are mainly by Nb, Nb 5Si 3, NbC forms.Its XRD figure spectrum as shown in Figure 5.
Embodiment 6
Nb-Si-Mo (at%) sample is imbedded Al 2O 3Carry out in+SiC+Al the powder from spreading sintering
With Nb, Si, the Mo powder is mixed with Nb: Si respectively: the Mo atomic ratio is 77: 18: 5, three kinds of composite powders of 72: 18: 10 and 69: 16: 15, ball milling 10h in planetary ball mill, ball-milling medium are alcohol, ratio of grinding media to material is 3: 1, and the stearic acid of adding 2wt% is as process control agent.Behind the sample drying behind the ball milling at the forming under the pressure of 300MPa.Sample after the moulding is imbedded Al 2O 3+ SiC+Al (mass ratio Al 2O 3: put into microwave cavity after SiC: Al=18: 80: 2) in the powder, be evacuated to and charge into mobile argon gas behind the 2Pa, under argon shield, carry out from spreading sintering.Start microwave source, heating rate is 10-40 ℃/min, 1450 ℃ of sintering temperatures, temperature retention time 30min.Sample is taken out in the cold back of stove.Sample after burning till is mainly by Nb, Nb 5Si 3And Nb 3Si forms.Its XRD figure spectrum as shown in Figure 6.
Embodiment 7
Nb-14Ti-18Si-10Cr-5Al-10Mo (at%) sample is imbedded Al 2O 3Carry out in+SiC+C the powder from spreading sintering
With Nb, Ti, Si, Cr, Al, the Mo powder is mixed with Nb: Ti: Si: Cr: Al respectively: the Mo atomic ratio is 43: 14: 18: 10: 5: 10 composite powder, ball milling 10h in planetary ball mill, ball-milling medium is an alcohol, and ratio of grinding media to material is 3: 1, and the stearic acid of adding 2wt% is as process control agent.Behind the sample drying behind the ball milling at the forming under the pressure of 300MPa.Sample after the moulding is imbedded Al 2O 3+ SiC+C (mass ratio Al 2O 3: put into microwave cavity after SiC: C=20: 78: 2) in the powder, be evacuated to and charge into mobile argon gas behind the 2Pa, under argon shield, carry out from spreading sintering.Start microwave source, heating rate is 10-40 ℃/min, 1450 ℃ of sintering temperatures, temperature retention time 30min.Sample is taken out in the cold back of stove.Sample after burning till is mainly by Nb, Nb 5Si 3, Nb 3Si, NbTi 4, Cr 3Mo forms.Its XRD figure spectrum as shown in Figure 7.
Whole process of preparation of the present invention is utilized aluminium powder and activated carbon powder and is vacuumized oxygen reaction remaining in the equipment of back, and has made full use of microwave sintering process and the synthetic advantage of self propagating high temperature, synthetic sample oxide-free, and preparation time is short, reacts completely.

Claims (7)

1. a microwave induced self propagating high temperature synthesizes Nb/Nb 5Si 3The method of composite, this method is made up of composition of raw materials and synthesis technique, described composition of raw materials comprises pure niobium powder and pure silicon powder, wherein, pure niobium powder and pure silicon powder proportioning are Nb-(5-37.5at.%) Si, also comprise: B, C, Al, Fe, Hf, W, Mo, V, among Ti and the Cr any one or two or more multiple alloy powders, at above-mentioned B, C, Al, any consumption is the 1-5at% of total raw material consumption in the alloy powder of Fe and Hf, W, Mo, V, any consumption is the 5-15at% of total raw material consumption among Ti and the Cr, and described synthesis technique comprises the steps:
(1) batching: at first each material powder in the composition of raw materials is mixed in proportion the polynary composite powder of preparation;
(2) grind: it is 800 purpose fine powders that above-mentioned polynary composite powder is ground to form granularity;
(3) moulding: make polynary composite powder after the above-mentioned grinding at the forming under the pressure of 100-300MPa;
(4) spread sintering certainly: molded material is put into microwave cavity and is carried out charging into mobile argon gas after vacuumizing in the microwave cavity when spreading sintering certainly from spreading sintering with microwave under argon shield.
2. a kind of microwave induced self propagating high temperature according to claim 1 synthesizes Nb/Nb 5Si 3The method of composite is characterized in that spreading in the sintering circuit certainly described, and heating rate is 10-100 ℃/min, spreads sintering temperature 1200-1500 ℃ certainly, and temperature retention time is no more than 30min.
3. a kind of microwave induced self propagating high temperature according to claim 2 synthesizes Nb/Nb 5Si 3The method of composite is characterized in that spreading in the sintering circuit certainly described, the low thermophase below 350 degree, and heating rate is 10-40 ℃/min, at the above hot stage of 350 degree, heating rate is that 40-100 ℃/min is to sintering temperature.
4. a kind of microwave induced self propagating high temperature according to claim 1 synthesizes Nb/Nb 5Si 3The method of composite is characterized in that spreading in the sintering circuit certainly described, and the sample after the moulding is imbedded Al 2O 3, put into microwave cavity behind the protection powder that mixes of SiC and Al and carry out from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 18wt%, SiC:80wt%, Al:2wt%.
5. a kind of microwave induced self propagating high temperature according to claim 1 synthesizes Nb/Nb 5Si 3The method of composite is characterized in that spreading in the sintering circuit certainly described, and the sample after the moulding is imbedded Al 2O 3, put into microwave cavity behind the protection powder that mixes of SiC and C and carry out from spreading sintering, the proportioning of above-mentioned protection powder is Al 2O 3: 20wt%, SiC:78wt%, C:2wt%.
6. a kind of microwave induced self propagating high temperature according to claim 1 synthesizes Nb/Nb 5Si 3The method of composite is characterized in that spreading in the sintering circuit certainly described, is evacuated to below the 2Pa in the microwave cavity.
7. a kind of microwave induced self propagating high temperature according to claim 1 synthesizes Nb/Nb 5Si 3The method of composite is characterized in that in described grinding step, adopts planetary ball mill to composite powder ball milling 2-48h, and ball-milling medium is an alcohol, ball material weight ratio 3: 1, and the stearic acid of adding 2wt% is as process control agent.
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