CN101168815A - Non-metal element alloyed sheet layer niobium-molybdenum-silicon-base in situ composite material and preparation method thereof - Google Patents
Non-metal element alloyed sheet layer niobium-molybdenum-silicon-base in situ composite material and preparation method thereof Download PDFInfo
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- CN101168815A CN101168815A CNA2007101787438A CN200710178743A CN101168815A CN 101168815 A CN101168815 A CN 101168815A CN A2007101787438 A CNA2007101787438 A CN A2007101787438A CN 200710178743 A CN200710178743 A CN 200710178743A CN 101168815 A CN101168815 A CN 101168815A
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Abstract
The invention discloses a non-metal element alloyed sheet layer niobium molybdenum silicon based insitu compound material and the preparation method thereof. The Nb-Mo-Si insitu compound material is composed of 30 to 87at percent Nb, 3 to 40at percent Mo and 10 to 30at percent Si. In order to enhance the intensity or the creep resistance of the Nb-Mo-Si insitu compound material at the high temperature of 1200 to 1500 DEG C, 0.1 to 10at percent B or 0.1 to 10at percent Ge can be added. The Nb-Mo-Si insitu compound material of the invention adopts light suspension area melting positioning coagulation method to be prepared, and the produced non-metal element alloyed insitu compound material has two phases of (Nb, Mo)ss and (Nb, Mo)5Si3, and has a sheet layer structure. The compression yield strength is 1200 to 2200MPa at 18 to 25 DEG C, and 300 to 1000MPa at 1200 to 1500 DEG C; the creep deformation amount is 0.5 to 1.0 percent under the conditions that the temperature is 1200DEG C, the stress is 170MPa and the creeping treatment is performed for 100 hours.
Description
Technical field
The present invention relates to a kind of niobium-molybdenum-silicon high-temperature alloy material, more particularly say, be meant a kind of laminated structure, non-metal element alloyed, niobium-molybdenum-silicon-base in situ composite material that has, and adopt the molten directional solidification process in light suspension zone to prepare niobium-molybdenum-silicon-base in situ composite material with laminated structure.
Background technology
The a large amount of use held the high high temperature alloy of warm ability in fields such as the energy, petrochemical complex, aerospace, for example the blade material of aero-turbine generally adopts nickel base superalloy, the use temperature of present state-of-the-art third generation nickel-base high-temperature single crystal alloy reaches 1150 ℃, yet this is near 1350 ℃ of the fusing points of nickel base superalloy, and it is little that nickel-base high-temperature single crystal alloy continues the space of development.For the further performance that improves turbine engine, and improve efficiency of combustion, reduce energy consumption and exhaust gas emission, must develop and hold the higher blade material of warm ability.
The binary niobium-silicon alloy that employing casting-heat treating method makes is by niobium sosoloid (Nb
Ss) and intermetallic compound Nb
5Si
3Two phase composites.Eutectic reaction: L → Nb at first takes place at 1920 ℃ in the binary niobium-silicon alloy
Ss+ Nb
3Eutectoid reaction: Nb takes place at 1 770 ℃ in Si then
3Si → Nb
Ss+ Nb
5Si
3, the Nb that obtains by two-step reaction
SsAnd Nb
5Si
3Two-phase is because the difficult control of complicated its form of reaction.
Use the method for physical vapor deposition can obtain metal niobium and Nb
5Si
3The laminated structure of two phase composites, but there is following problem in the niobium silicon composite that this method obtains: and crystal grain is tiny, a little less than the creep resistance; The two-phase non-equilibrium thermodynamics, tissue is unstable; Preparation technology is complicated, and cost is higher.
Summary of the invention
Nb-Mo-Si in-situ composite of the present invention is made up of the niobium (Nb) of 30～87at%, the molybdenum (Mo) of 3～40at% and the silicon (Si) of 10～30at%.Its adopted light floating zone melting directional freeze preparation, the Nb-Mo-Si in-situ composite that makes have (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase, and the lamella percent by volume is arranged greater than 50% laminated structure.The Nb-Mo-Si in-situ composite is 1200～2000MPa 18～25 ℃ compressive strength, is 300～900MPa 1200～1500 ℃ compressive strengths; At 1200 ℃, stress is that 170MPa, creep are handled under the condition of 100 h, and the creep strain amount is 0.8～1.0%.
A kind of non-metal element alloyed Nb-Mo-Si in-situ composite of the present invention is to improve the Nb-Mo-Si-B alloy 1200～1500 ℃ of pyritous intensity by the boron (B) that adds 0.1～10at% in the Nb-Mo-Si in-situ composite.Adopted light floating zone melting directional freeze preparation, the Nb-Mo-Si-B in-situ composite that makes have (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase, and B be solid-solubilized in (Nb, Mo)
5Si
3Mutually, has the lamella percent by volume greater than 50% laminated structure.
A kind of non-metal element alloyed Nb-Mo-Si in-situ composite of the present invention is to improve the Nb-Mo-Si-Ge alloy 1200～1500 ℃ of pyritous creep resistances by the germanium (Ge) that adds 0.1～10at% in the Nb-Mo-Si in-situ composite.Adopted light floating zone melting directional freeze preparation, the Nb-Mo-Si-Ge in-situ composite that makes have (Nb, Mo)
Ss(Nb, Mo)
5(Si, Ge)
3Two-phase, and have the lamella percent by volume greater than 50% laminated structure.
Description of drawings
Figure 1A is Nb
72Mo
10Si
18Alloy longitudinal profile back scattering photo.
Figure 1B is Nb
72Mo
10Si
18Alloy horizontal section back scattering photo.
Fig. 2 is Nb
70Mo
10Si
18B
2Alloy longitudinal profile back scattering photo.
Fig. 3 is Nb
72Mo
10Si
16Ge
2Alloy longitudinal profile back scattering photo.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Nb-Mo-Si in-situ composite of the present invention is made up of the niobium (Nb) of 30～87at%, the molybdenum (Mo) of 3～40at% and the silicon (Si) of 10～30at%.The Nb-Mo-Si in-situ composite have (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase.
Nb-Mo-Si-B in-situ composite of the present invention is on Nb-Mo-Si in-situ composite basis, in order to improve it 1200～1500 ℃ of pyritous intensity, has added the boron (B) of 0.1～10at%.Make the Nb-Mo-Si-B in-situ composite have (Nb, Mo)
SsPhase (Nb sosoloid mutually in Mo partly substitute Nb) and (Nb, Mo)
5Si
3Phase (Nb
5Si
3Mutually middle Mo partly substitutes Nb), and B be solid-solubilized in (Nb, Mo)
5Si
3Mutually.This Nb-Mo-Si-B in-situ composite is 1200～2200MPa at 18～25 ℃ compression yield strength, is 300～1000MPa at 1200～1500 ℃ compression yield strengths.
Nb-Mo-Si-Ge in-situ composite of the present invention is on Nb-Mo-Si in-situ composite basis, in order to improve it 1200～1500 ℃ of pyritous creep resistances, has added the germanium (Ge) of 0.1～10at%.Make the Nb-Mo-Si-Ge in-situ composite have (Nb, Mo)
SsPhase (Nb sosoloid mutually in Mo partly substitute Nb) and (Nb, Mo)
5(Si, Ge)
3Phase (Nb
5Si
3Mutually middle Mo partly substitutes Nb, and Ge partly substitutes Si).This Nb-Mo-Si-Ge in-situ composite is that 170MPa, creep are handled under the condition of 100h at 1200 ℃, stress, and the creep strain amount is 0.5～1.0%.
One, the Nb-Mo-Si in-situ composite (alloy) of film-making layer structure
A kind of method that adopts light floating zone melting directional freeze to prepare the Nb-Mo-Si in-situ composite includes the following step:
The first step: taking by weighing purity by Nb-Mo-Si target component proportioning is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si) is stand-by;
Second step: the above-mentioned target component raw material that takes by weighing is put into non-consumable arc furnace, be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700～3000 ℃ of following meltings of smelting temperature 2～5 times, makes alloy pig;
The 3rd step: (A) alloy pig that second step was made adopts the line cutting processing to obtain alloy charge bar and base rod, it is inserted in the light floating zone melting stove then, and charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa, charging into flow velocity is 1～2L/min argon gas, the mobile argon gas plays the refrigerative effect, forms suitable temperature gradient.Charge bar and base rod keep rotation, and sense of rotation is opposite, and speed of rotation is 0～50r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 60～100 ℃/min, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 0.5～10mm/h, thermograde 100～200K/cm, pull 5～20h, directional freeze finishes, and makes the Nb-Mo-Si in-situ composite (alloy) with laminated structure.
Adopt JSM-5600HV/LV type scanning electronic microscope to do the microtexture analysis the above-mentioned Nb-Mo-Si alloy that makes, its have (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase and two-phase have laminated structure.Adopting day island proper Tianjin high temperature experimental machine to carry out stress under compression-strain testing to the Nb-Mo-Si alloy, is 1200～2000MPa at the compression yield strength of room temperature (18～25 ℃), is 300～900MPa at 1200～1500 ℃ compression yield strengths.Adopting Shenzhen to think carefully that newly (according to GB/T2039-1997) carries out creep test on the GWT304 type creep test machine of company to the Nb-Mo-Si alloy, is that 170MPa, creep are handled under the condition of 100h at 1200 ℃, stress, and the creep strain amount is 0.8～1.0%.
Two, Nb-Mo-Si-B in-situ composite (alloy) the first step of film-making layer structure: taking by weighing purity by Nb-Mo-Si-B target component proportioning is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si), purity are that 99.99% boron (B) is stand-by; Second step: the above-mentioned target component raw material that takes by weighing, boron (B) are put into non-consumable arc furnace, be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700～3000 ℃ of following meltings of smelting temperature 2～5 times, makes alloy pig;
The 3rd step: (A) alloy pig that second step was made adopts the line cutting processing to obtain alloy charge bar and base rod, it is inserted in the light floating zone melting stove then, and charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa, charging into flow velocity is 1～2L/min argon gas, the mobile argon gas plays the refrigerative effect, forms suitable temperature gradient.Charge bar and base rod keep rotation, and sense of rotation is opposite, and speed of rotation is 0～50r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 60～100 ℃/min, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 0.5～10mm/h, thermograde 100～200K/cm,, pull 5～20h, directional freeze finishes, and makes the Nb-Mo-Si-B in-situ composite (alloy) with laminated structure.
Adopt JSM-5600HV/LV type scanning electronic microscope to do the microtexture analysis the above-mentioned Nb-Mo-Si-B alloy that makes, its have (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase, and B be solid-solubilized in (Nb, Mo)
5Si
3Mutually, two-phase has laminated structure.Adopting day island proper Tianjin high temperature experimental machine to carry out stress under compression-strain testing to the Nb-Mo-Si-B alloy, is 1200～2200MPa at the compression yield strength of room temperature (18～25 ℃), is 300～1000MPa at 1200～1500 ℃ compression yield strengths.
Three, the Nb-Mo-Si-Ge in-situ composite (alloy) of film-making layer structure
The first step: taking by weighing purity by Nb-Mo-Si-Ge target component proportioning is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si), purity are that 99.99% germanium (Ge) is stand-by;
Second step: the above-mentioned target component raw material that takes by weighing, germanium (Ge) are put into non-consumable arc furnace, be evacuated to 1 * 10
-3Pa～5 * 10
-4Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700～3000 ℃ of following meltings of smelting temperature 2～5 times, makes alloy pig;
The 3rd step: (A) alloy pig that second step was made adopts the line cutting processing to obtain alloy charge bar and base rod, it is inserted in the light floating zone melting stove then, and charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 1 * 10
-3Pa～5 * 10
-4Pa, charging into flow velocity is 1～2L/min argon gas, the mobile argon gas plays the refrigerative effect, forms suitable temperature gradient.Charge bar and base rod keep rotation, and sense of rotation is opposite, and speed of rotation is 0～50r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 60～100 ℃/min, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 0.5～10mm/h, thermograde 100～200K/cm,, pull 5～20h, directional freeze finishes, and makes the Nb-Mo-Si-Ge in-situ composite (alloy) with laminated structure.
Adopt JSM-5600HV/LV type scanning electronic microscope to do the microtexture analysis the above-mentioned Nb-Mo-Si-Ge alloy that makes, its have (Nb, Mo)
Ss(Nb, Mo)
5(Si, Ge)
3Two-phase, and two-phase has laminated structure.Adopt Shenzhen to think carefully that newly (according to GB/T2039-1997) carries out creep test on the GWT304 type creep test machine of company (SANS) to the Nb-Mo-Si-Ge alloy, at 1200 ℃, stress is that 170MPa, creep are handled under the condition of 100h, and the creep strain amount is 0.5～1.0%.
Embodiment 1:The Nb of film-making layer structure
72Mo
10Si
18Alloy
The first step: press Nb
72Mo
10Si
18It is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si) is stand-by that proportioning takes by weighing purity;
Second step: the above-mentioned raw material that takes by weighing is put into non-consumable arc furnace, be evacuated to 5 * 10
-4Pa charges into high-purity argon gas to 0.5 * 10
5Pa 3000 ℃ of following meltings of smelting temperature 4 times, makes alloy pig;
The 3rd step: (A) adopt wire cutting method, go on foot the base rod that cuts φ 9mm * 90mm alloy charge bar and φ 9mm * 40mm in the alloy pig that makes with second, it is inserted in the light floating zone melting stove then, charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 5 * 10
-4Pa, charging into flow velocity is 2L/min argon gas (charging into argon gas is 1 normal atmosphere), and charge bar is opposite with base rod sense of rotation, and speed of rotation is 10r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 60 ℃/minute, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 5mm/h, thermograde 200K/cm makes the Nb with laminated structure behind pull 8 h
72Mo
10Si
18Alloy.
The method that adopts the line cutting is with the above-mentioned Nb with laminated structure that makes
72Mo
10Si
18Alloy bar material longitudinally center is cut open, and polishes with waterproof abrasive paper, with diamond paste and clear water polishing, is microtexture analysis, Nb with JSM-5600HV/LV type scanning electronic microscope then again
72Mo
10Si
18In the alloy by (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two phase composites.Through the above-mentioned Nb that makes
72Mo
10Si
18No matter alloy is vertical (shown in Figure 1A), and still laterally (shown in Figure 1B) all has laminated structure.
Adopt wire cutting method, at the above-mentioned Nb that makes
72Mo
10Si
18Alloy cuts the right cylinder of φ 3mm * 5mm as the Mechanics Performance Testing sample, adopts day island proper Tianjin high temperature experimental machine to carry out stress under compression-strain testing, and compressive strain speed is 3 * 10
-4s
-1, vacuum tightness is 1 * 10
-3Pa.Experimental temperature is room temperature, 1200 ℃.The right cylinder sample carries out surface finish with 1000#SiC sand paper before experiment.Rate of heating is 10 ℃/minute during the high temperature experiment, keeps carrying out in 10 minutes compression experiment, the Nb that makes behind the arrival design temperature again
72Mo
10Si
18The compression yield strength of alloy material in the time of 25 ℃ is 1720MPa, and the compression yield strength in the time of 1200 ℃ is 842MPa.Creep test is to think carefully newly that in Shenzhen (according to GB/T2039-1997) carries out on the GWT304 type creep test machine of company, is under the condition of 170MPa at 1200 ℃, stress, Nb
72Mo
10Si
18Alloy is through the 100h creep, and its deflection is 0.96%.
Adopt the preparation method identical with embodiment 1, make the Nb-Mo-Si alloy with laminated structure of heterogeneity, its Specifeca tion speeification is as shown in the table:
| Alloying constituent (at%) | Probe temperature (℃) | Compression yield strength (MPa) | 1200 ℃, stress are under the condition of 170MPa, through the deflection of 100h creep |
| Nb 62Mo 20Si 18 | 25 | 1783 | - |
| 1200 | 864 | 0.92％ | |
| Nb 65Mo 10Si 25 | 25 | 1942 | - |
| 1200 | 890 | 0.84％ | |
| Nb 50Mo 30Si 20 | 25 | 1883 | - |
| 1200 | 882 | 0.89％ |
Embodiment 2:The Nb of film-making layer structure
70Mo
10Si
18B
2Alloy
The first step: press Nb
70Mo
10Si
18B
2It is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si), purity are that 99.99% boron (B) is stand-by that proportioning takes by weighing purity;
Second step: the above-mentioned raw material that takes by weighing is put into non-consumable arc furnace, be evacuated to 8 * 10
-4Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700 ℃ of following meltings of smelting temperature 5 times, makes alloy pig;
The 3rd step: (A) adopt wire cutting method, go on foot the base rod that cuts φ 9mm * 90mm alloy charge bar and φ 9mm * 40mm in the alloy pig that makes with second, it is inserted in the light floating zone melting stove then, charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 8 * 10
-4Pa, charging into flow velocity is 1.8L/min argon gas (charging into argon gas is 1 normal atmosphere), and charge bar is opposite with base rod sense of rotation, and speed of rotation is 20r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 80 ℃/minute, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 8mm/h, thermograde 180K/cm, pull 6h makes the Nb with laminated structure
70Mo
10Si
18B
2Alloy.
The method that adopts the line cutting is with the above-mentioned Nb with laminated structure that makes
70Mo
10Si
18B
2Alloy bar material longitudinally center is cut open, and polishes with waterproof abrasive paper, with diamond paste and clear water polishing, is microtexture analysis, Nb with JSM-5600HV/LV type scanning electronic microscope then again
70Mo
10Si
18B
2Have in the alloy (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase, and B be solid-solubilized in (Nb, Mo)
5Si
3Mutually, and has laminated structure, referring to shown in Figure 2.
Adopt wire cutting method, at the above-mentioned Nb that makes
72Mo
10Si
18Alloy cuts the right cylinder of φ 3mm * 5mm as the Mechanics Performance Testing sample, adopts day island proper Tianjin high temperature experimental machine to carry out stress under compression-strain testing, and compressive strain speed is 3 * 10
-4s
-1, vacuum tightness is 1 * 10
-3Pa.Experimental temperature is room temperature, 1200 ℃.The right cylinder sample carries out surface finish with 1000#SiC sand paper before experiment.Rate of heating is 10 ℃/minute during the high temperature experiment, keeps carrying out in 10 minutes compression experiment behind the arrival design temperature again.Creep test is to think carefully that newly (according to GB/T2039-1997) carries out on the GWT304 type creep test machine of company.The above-mentioned Nb that makes
72Mo
10Si
18The compression yield strength of alloy in the time of 25 ℃ is 1780MPa, and the compression yield strength in the time of 1500 ℃ is 390MPa.At 1200 ℃, stress is under the condition of 170MPa, Nb
72Mo
10Si
18Alloy is 0.76% through 100h creep strain amount.
Adopt the preparation method identical with embodiment 2, make the Nb-Mo-Si-B alloy with laminated structure of heterogeneity, its Specifeca tion speeification is as shown in the table:
| Alloying constituent | Probe temperature (℃) | Compression yield strength (MPa) | |
| Nb-Mo-Si(at％) | B(at％) | ||
| Nb 62Mo 20Si 18 | 2 | 25 | 1822 |
| 1200 | 883 | ||
| Nb 63Mo 12Si 25 | 2 | 25 | 1980 |
| 1200 | 924 | ||
| Nb 50Mo 30Si 20 | 1 | 25 | 1928 |
| 1200 | 902 | ||
| Nb 47Mo 35Si 18 | 5 | 1200 | 912 |
| Nb 47Mo 35Si 18 | 10 | 1200 | 925 |
Embodiment 3:The Nb of film-making layer structure
72Mo
10Si
16Ge
2Alloy
The first step: press Nb
72Mo
10Si
16It is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si), purity are that 99.99% germanium (Ge) is stand-by that the Ge2 proportioning takes by weighing purity;
Second step: the above-mentioned raw material that takes by weighing is put into non-consumable arc furnace, be evacuated to 8 * 10
-4Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700 ℃ of following meltings of smelting temperature 5 times, makes alloy pig;
The 3rd step: (A) adopt wire cutting method, go on foot the base rod that cuts φ 9mm * 90mm alloy charge bar and φ 9mm * 40mm in the alloy pig that makes with second, it is inserted in the light floating zone melting stove then, charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 8 * 10
-4Pa, charging into flow velocity is 1.6L/min (charging into argon gas is 1 normal atmosphere), and charge bar is opposite with base rod sense of rotation, and speed of rotation is 40r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 80 ℃/minute, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 3mm/h, thermograde 160K/cm, the alloy bar material speed of rotation is 40r/min, directional freeze 15h makes the Nb with laminated structure
72Mo
10Si
16Ge
2Alloy.
The method that adopts the line cutting is with the above-mentioned Nb with laminated structure that makes
72Mo
10Si
16Ge
2Alloy bar material longitudinally center is cut open, and polishes with waterproof abrasive paper, with diamond paste and clear water polishing, is microtexture analysis, Nb with JSM-5600HV/LV type scanning electronic microscope then again
72Mo
10Si
16Ge
2Have in the alloy (Nb, Mo)
Ss(Nb, Mo)
5(Si, Ge)
3Two-phase, and have laminated structure, referring to shown in Figure 3.
Adopt wire cutting method, at the above-mentioned Nb that makes
72Mo
10Si
16Ge
2Alloy cuts the right cylinder of φ 3mm * 5mm as the Mechanics Performance Testing sample, and creep test is to think carefully newly that in Shenzhen (according to GB/T2039-1997) carries out on the GWT304 type creep test machine of company.The above-mentioned Nb that makes
72Mo
10Si
16Ge
2Alloy material is that 170MPa, creep are handled under the condition of 100h at 1200 ℃, stress, and the creep strain amount is 0.74%.
Adopt the preparation method identical with embodiment 3, make the Nb-Mo-Si-Ge alloy with laminated structure of heterogeneity, its Specifeca tion speeification is as shown in the table:
| Alloying constituent | 1200 ℃, stress are under the condition of 170MPa, alloy 100h creep strain amount | |
| Nb-Mo-Si(at％) | Ge(at％) | |
| Nb 60Mo 20Si 20 | 2 | 0.68％ |
| Nb 63Mo 12Si 25 | 2 | 0.57％ |
| Nb 50Mo 20Si 30 | 2 | 0.62％ |
| Nb 50Mo 30Si 20 | 1 | 0.64％ |
| Nb 50Mo 30Si 20 | 5 | 0.62％ |
| Nb 50Mo 30Si 20 | 10 | 0.60％ |
Claims (10)
1. non-metal element alloyed sheet layer niobium-molybdenum-silicon-base in situ composite material, it is characterized in that: the Nb-Mo-Si in-situ composite is made up of the niobium (Nb) of 30～87at%, the molybdenum (Mo) of 3～40at% and the silicon (Si) of 10～30at%.
2. niobium-molybdenum-silicon-base in situ composite material according to claim 1 is characterized in that: the boron (B) that adds 0.1～10at% in the Nb-Mo-Si in-situ composite improves the Nb-Mo-Si in-situ composite 1200～1500 ℃ of pyritous intensity.
3. niobium-molybdenum-silicon-base in situ composite material according to claim 1 is characterized in that: the germanium (Ge) that adds 0.1～10at% in the Nb-Mo-Si in-situ composite improves the Nb-Mo-Si in-situ composite 1200～1500 ℃ of pyritous creep resistances.
4. niobium-molybdenum-silicon-base in situ composite material according to claim 1 is characterized in that: the Nb-Mo-Si in-situ composite have (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase; At 18～25 ℃ compression yield strengths is 1200～2000MPa, is 300～900MPa at 1200～1500 ℃ compression yield strengths; At 1200 ℃, stress is that 170MPa, creep are handled under the condition of 100 h, and the creep strain amount is 0.8～1.0%.
5. niobium-molybdenum-silicon-base in situ composite material according to claim 2 is characterized in that: the Nb-Mo-Si-B in-situ composite have (Nb, Mo)
Ss(Nb, Mo)
5Si
3Two-phase, and B be solid-solubilized in (Nb, Mo)
5Si
3Mutually, being 1200～2200MPa at 18～25 ℃ compression yield strengths, is 300～1000MPa at 1200～1500 ℃ compression yield strengths.
6. niobium-molybdenum-silicon-base in situ composite material according to claim 3 is characterized in that: the Nb-Mo-Si-Ge in-situ composite have (Nb, Mo)
Ss(Nb, Mo)
5(Si, Ge)
3Two-phase is that 170MPa, creep are handled under the condition of 100h at 1200 ℃, stress, and the creep strain amount is 0.5～1.0%.
7. according to claim 1,2 or 3 described niobium-molybdenum-silicon-base in situ composite material, it is characterized in that: the in-situ composite composition has Nb
72Mo
10Si
18, Nb
70Mo
10Si
18B
2Perhaps Nb
72Mo
10Si
16Ge
2
8. method that adopts light floating zone melting directional freeze to prepare niobium-molybdenum-silicon-base in situ composite material as claimed in claim 1 is characterized in that the following step is arranged:
The first step: taking by weighing purity by Nb-Mo-Si target component proportioning is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si) is stand-by;
Second step: the above-mentioned target component raw material that takes by weighing is put into non-consumable arc furnace, be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700～3000 ℃ of following meltings of smelting temperature 2～5 times, makes alloy pig;
The 3rd step: (A) alloy pig that second step was made adopts the line cutting processing to obtain alloy charge bar and base rod, it is inserted in the light floating zone melting stove then, and charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa, charging into flow velocity is 1～2L/min argon gas, the mobile argon gas plays the refrigerative effect, forms suitable temperature gradient.Charge bar and base rod keep rotation, and sense of rotation is opposite, and speed of rotation is 0～50r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 60～100 ℃/min, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 0.5～10mm/h, thermograde 100～200K/cm, pull 5～20h, directional freeze finishes, and makes the Nb-Mo-Si in-situ composite with laminated structure.
9. method that adopts light floating zone melting directional freeze to prepare niobium-molybdenum-silicon-base in situ composite material as claimed in claim 2 is characterized in that the following step is arranged:
The first step: taking by weighing purity by Nb-Mo-Si-B target component proportioning is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si), purity are that 99.99% boron (B) is stand-by;
Second step: the above-mentioned target component raw material that takes by weighing, boron (B) are put into non-consumable arc furnace, be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700～3000 ℃ of following meltings of smelting temperature 2～5 times, makes alloy pig;
The 3rd step: (A) alloy pig that second step was made adopts the line cutting processing to obtain alloy charge bar and base rod, it is inserted in the light floating zone melting stove then, and charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa, charging into flow velocity is 1～2L/min argon gas, the mobile argon gas plays the refrigerative effect, forms suitable temperature gradient.Charge bar and base rod keep rotation, and sense of rotation is opposite, and speed of rotation is 0～50r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 60～100 ℃/min, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 0.5～10mm/h, thermograde 100～200K/cm, pull 5～20h, directional freeze finishes, and makes the Nb-Mo-Si-B in-situ composite with laminated structure.
10. method that adopts light floating zone melting directional freeze to prepare niobium-molybdenum-silicon-base in situ composite material as claimed in claim 3 is characterized in that the following step is arranged:
The first step: taking by weighing purity by Nb-Mo-Si-Ge target component proportioning is that 99.99% niobium (Nb), purity are that 99.99% molybdenum (Mo), purity are that 99.99% silicon (Si), purity are that 99.99% germanium (Ge) is stand-by;
Second step: the above-mentioned target component raw material that takes by weighing, germanium (Ge) are put into non-consumable arc furnace, be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2700～3000 ℃ of following meltings of smelting temperature 2～5 times, makes alloy pig;
The 3rd step: (A) alloy pig that second step was made adopts the line cutting processing to obtain alloy charge bar and base rod, it is inserted in the light floating zone melting stove then, and charge bar is suspended on upper boom, and the base rod is fixed on lower beam;
(B) be evacuated to 5 * 10
-4Pa～1 * 10
-3Pa, charging into flow velocity is 1～2L/min argon gas, the mobile argon gas plays the refrigerative effect, forms suitable temperature gradient.Charge bar and base rod keep rotation, and sense of rotation is opposite, and speed of rotation is 0～50r/min.
(C) charge bar is begun heating, Heating temperature raises gradually, and heat-up rate is 60～100 ℃/min, until the charge bar fusing, then charge bar is docked with the base rod.The beginning pull, drawing velocity is 0.5～10mm/h, thermograde 100～200K/cm, pull 5～20h, directional freeze finishes, and makes the Nb-Mo-Si-Ge in-situ composite with laminated structure.
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