CN107760952A - A kind of Mo Si C alloy bars and preparation method thereof - Google Patents
A kind of Mo Si C alloy bars and preparation method thereof Download PDFInfo
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- CN107760952A CN107760952A CN201711091836.7A CN201711091836A CN107760952A CN 107760952 A CN107760952 A CN 107760952A CN 201711091836 A CN201711091836 A CN 201711091836A CN 107760952 A CN107760952 A CN 107760952A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The invention discloses a kind of Mo Si C alloy bars, it is made up of the raw material of following atomic percent：Silicon 15%~25%, carbon 15%~35%, surplus are molybdenum and inevitable impurity.In addition, the invention also discloses the method for preparing the Mo Si C alloy bars, this method is：First, it will be dried after material powder ball milling, obtain mixed-powder；2nd, blank is obtained by mixed-powder is compressing, sintering processes obtain Mo Si C alloy sintered bodies；3rd, Mo Si C alloys sintered body obtains Mo Si C alloy ingot castings through electronic torch melting, cuts into semi-finished product bar；4th, semi-finished product bar obtains Mo Si C alloy bars through electron beam zone melting.Mo Si C alloy bars of the present invention have the characteristics of purity is high low with oxygen mass content, have high hardness and tensile strength, excellent fatigue behaviour and elevated temperature strength, have broad application prospects under hyperthermal environments.
Description
Technical field
The invention belongs to field of alloy preparation technology, and in particular to a kind of Mo-Si-C alloy bar materials and preparation method thereof.
Background technology
With the development of aeronautical and space technology, the raising of various course of new aircraft flying distances and flying speed, it is desirable to send out
Motivation has an high regard for when operating efficiency with higher, and people propose more to lightweight, high-strength and oxidation resistant high-temperature structural material
Carry out higher requirement.And the nickel base superalloy used in available engine is by its own fusing point due to being limited, in temperature in use
Limit is only 1100 DEG C.Therefore, the hyperthermal material for developing replacement nickel based super alloy is imperative.Molybdenum alloy is in the 1950s
Just once it is widely studied as the candidate material of Aero-Space, nuclear engineering and aircraft engine.Although molybdenum alloy is being processed
Forming property, density and fusing point etc. are very tempting, but its poor fatigue strength turns into it as high-temperature structural material application
Major obstacle.Meanwhile when temperature in use is more than 1100 DEG C, the mechanical behavior under high temperature of molybdenum alloy is remarkably decreased.Add in molybdenum
Additional element can form the high molybdenum alloy of alloy concentrations, and its mechanical behavior under high temperature makes moderate progress, and processing characteristics is good, therefore
As high-temperature structural material.However, the elevated temperature strength of these molybdenum alloy materials difference, is restricted its application, this is due to this
Long-time Dynamic Thermal/couple of force of a little materials under hyperthermal environments is closed under load-up condition, the existing strengthened mechanism of material itself
Effect may be lost under high-temperature service.Therefore, although traditional molybdenum alloy mechanical behavior under high temperature can be made by alloying
A certain degree of improvement is obtained with fatigue strength, but greatly improve its mechanical property to make it on high thrust-weight ratio engine of future generation
The limited promise being applied.Therefore, in order to meet national defense industry and space flight and aviation technology development needs, it is necessary to prepare new
Superhigh temperature structural material.In addition, with the rapid development of modern science and technology, use of all trades and professions to refractory metal material is increasingly
Extensively, higher and higher requirement is also accordingly proposed to its performance.High-performance refractory metal alloy material must be developed as tip
The development in field provides material foundation.
The content of the invention
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of Mo-Si-C
Alloy bar material.The quality purity of the alloy bar material is 99.5%~99.9%, the mass content of impurity oxygen is 20ppm~40ppm,
Room temperature tensile intensity is 1120MPa~1680MPa, Rockwell hardness (HRC) is 60~70, through 5 × 107After secondary cycling fatigue experiment
Fatigue strength be 510MPa~680MPa, 1500 DEG C of tensile strength are 310MPa~420MPa, thus prove the Mo-Si-C close
Golden bar has the characteristics of purity is high low with oxygen mass content, and has high hardness and tensile strength, excellent fatigue
Performance and elevated temperature strength, have broad application prospects under hyperthermal environments.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of Mo-Si-C alloy bar materials, its feature
It is, is made up of the raw material of following atomic percent：Silicon 15%~25%, carbon 15%~35%, surplus is for molybdenum and unavoidably
Impurity.
Above-mentioned a kind of Mo-Si-C alloy bar materials, it is characterised in that be made up of the raw material of following atomic percent：Silicon
18%~20%, carbon 18%~30%, surplus is molybdenum and inevitable impurity.
Above-mentioned a kind of Mo-Si-C alloy bar materials, it is characterised in that be made up of the raw material of following atomic percent：Silicon
20%, carbon 25%, surplus is molybdenum and inevitable impurity.
In addition, present invention also offers a kind of method for preparing above-mentioned Mo-Si-C alloy bar materials, it is characterised in that including
Following steps：
It is 200r/ in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
Min~400r/min, ratio of grinding media to material are (5~15):Ball milling 20h~40h under conditions of 1, dry after ball milling, obtain under vacuum
To mixed-powder；The volume of the absolute ethyl alcohol be silica flour, 1~3 times of carbon dust and molybdenum powder gross mass, the list of absolute ethyl alcohol volume
Position is mL, and the unit of silica flour, carbon dust and molybdenum powder gross mass is g；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering
In stove, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sinterings is obtained after furnace cooling
Body；The temperature of the sintering processes is 2000 DEG C~2400 DEG C, and the time is 1h~3h；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than in vacuum
1×10-3Electronic torch melting 2~4 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots after cooling, then by the Mo-Si-C
Alloy cast ingot is cut into semi-finished product bar；The melting electric current of the electronic torch melting is 2A~4A, and melting voltage is 35kV
~75kV；
Step 4: semi-finished product bar described in step 3 are carried out with polishing removes surface scale, by described half after polishing
Finished product bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloys are obtained after cooling
Bar；The melting electric current of the electron beam zone melting is 3A~7A, and melting voltage is 40kV~60kV.
Above-mentioned method, it is characterised in that the quality purity of silica flour described in step 1 is not less than 99.5%, the carbon dust
Quality purity be not less than 99.5%, the quality purity of the molybdenum powder is not less than 99.5%.
Above-mentioned method, it is characterised in that the temperature of sintering processes described in step 2 is 2100 DEG C~2300 DEG C, the time
For 1.5h~2.5h.
Above-mentioned method, it is characterised in that the temperature of the sintering processes is 2200 DEG C, time 2h.
Above-mentioned method, it is characterised in that the temperature dried described in step 1 is 80 DEG C~90 DEG C.
The present invention has advantages below compared with prior art：
1st, Mo-Si-C alloy bar materials of the present invention have the characteristics of purity is high low with oxygen mass content, improve in superhigh temperature
The reliability used under environment.
2nd, the present invention uses ball mill mechanical alloying molybdenum powder, silica flour and carbon dust, first, making three kinds of powder stock mixing equal
It is even, second, can make that three kinds of powder stocks are pre-alloyed, and this not only reduces sintering temperature, it is often more important that promote molybdenum powder,
The Mo of silica flour and carbon dust reaction generation with complex crystals structure5SiC2Alloy phase.Mo5SiC2With high-melting-point, high rigidity and low
The characteristics of density, and possess high elevated temperature strength and high temperature creep property.
3rd, the technical process of electronic torch melting reduces impurity oxygen in Mo-Si-C alloy sintered compacts and other in the present invention
The content of impurity element, condition is created to carry out electron beam zone melting in next step, wherein during electron beam zone melting
Depth has purified bar, and gaseous impurity and other impurities content are very low in the Mo-Si-C alloy bar materials being prepared.
4th, using the composition design and preparation technology of optimization Mo-Si-C alloy bar materials are prepared, the alloy bar in the present invention
The quality purity of material is 99.5%~99.9%, the mass content of impurity oxygen is 20ppm~40ppm, and room temperature tensile intensity is
1120MPa~1680MPa, Rockwell hardness (HRC) are 60~70, through 5 × 107Fatigue strength after secondary cycling fatigue experiment is
510MPa~680MPa, 1500 DEG C of tensile strength are 310MPa~420MPa.
Technical scheme is described in further detail below by drawings and examples.
Brief description of the drawings
Fig. 1 is the metallograph of Mo-Si-C alloy bar materials prepared by the embodiment of the present invention 1.
Fig. 2 is the XRD spectra of Mo-Si-C alloy bar materials prepared by the embodiment of the present invention 1.
Embodiment
Embodiment 1
The present embodiment Mo-Si-C alloy bar materials are made up of the raw material of following atomic percent：Silicon 20%, carbon 25%, surplus
For molybdenum and inevitable impurity.
The method that the present embodiment prepares Mo-Si-C alloy bar materials comprises the following steps：
It is 300r/ in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
Mim, ratio of grinding media to material are calculated as 10 in mass ratio:Ball milling 30h under conditions of 1, dry after ball milling, mixed under 85 DEG C of vacuum conditions
Powder；The volume of the absolute ethyl alcohol is 2 times of silica flour, carbon dust and molybdenum powder quality sum, and the unit of absolute ethyl alcohol volume is mL,
The unit of silica flour, carbon dust and molybdenum powder gross mass is g；The quality purity of the silica flour is not less than 99.5%, the quality of the carbon dust
Purity is not less than 99.5%, and the quality purity of the molybdenum powder is not less than 99.5%；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering
In stove, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sinterings is obtained after furnace cooling
Body；The temperature of the sintering processes is 2200 DEG C, and time 2h, the blank is that cross sectional dimensions is 50mm (length) × 50mm
The strip-shaped blank of (width)；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than in vacuum
1×10-3Electronic torch melting 3 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots, then adopt the Mo-Si-C alloy cast ingots
Semi-finished product bar is cut into electric spark wire cutting method, the cross-sectional diameter of the bar is 25mm, and length is
850mm；The melting electric current of the electronic torch melting is 3A, and melting voltage is 55kV；
Step 4: to semi-finished product bar described in step 3 carry out polishing remove surface scale, then will it is described partly into
Product bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloy bars are obtained after cooling
Material；The melting electric current of the electron beam zone melting is 5A, and melting voltage is 50kV.
Fig. 1 is the metallograph of Mo-Si-C alloy bar materials manufactured in the present embodiment, from figure 1 it appears that the present embodiment
The Mo-Si-C alloy bar material crystal boundaries of preparation are clear-cut, crystal grain in etc. shaft-like, without visible micro-crack and it is empty the defects of,
The size of average crystal grain is about 800 μm.Fig. 2 is the XRD spectra of Mo-Si-C alloy bar materials manufactured in the present embodiment, can from Fig. 2
To find out, there is not Mo, Si and C diffraction maximum in XRD spectra, shows that Mo, Si and C almost participate in reaction completely, generates master
Contain Mo5SiC2The bar of alloy phase；The quality purity of Mo-Si-C alloy bar materials manufactured in the present embodiment is 99.9%, impurity
The mass content of oxygen is 20ppm, and room temperature tensile intensity is 1679MPa, Rockwell hardness (HRC) is 70, through 5 × 107Secondary circulation is tired
Fatigue strength after labor experiment is 679MPa, and 1500 DEG C of tensile strength are 420MPa.
Embodiment 2
The present embodiment Mo-Si-C alloy bar materials are made up of the raw material of following atomic percent：Silicon 25%, carbon 35%, surplus
For molybdenum and inevitable impurity.
The method that the present embodiment prepares Mo-Si-C alloy bar materials comprises the following steps：
It is 400r/ in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
Mim, ratio of grinding media to material are calculated as 15 in mass ratio:Ball milling 40h under conditions of 1, dry after ball milling, mixed under 90 DEG C of vacuum condition
Close powder；The volume of the absolute ethyl alcohol is 3 times of silica flour, carbon dust and molybdenum powder gross mass, and the unit of absolute ethyl alcohol volume is mL,
The unit of silica flour, carbon dust and molybdenum powder gross mass is g；The quality purity of the silica flour is not less than 99.5%, the quality of the carbon dust
Purity is not less than 99.5%, and the quality purity of the molybdenum powder is not less than 99.5%；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering
In stove, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sinterings is obtained after furnace cooling
Body；The temperature of the sintering processes is 2400 DEG C, and time 3h, the blank is that cross sectional dimensions is 50mm (length) × 50mm
The strip-shaped blank of (width)；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than in vacuum
1×10-3Electronic torch melting 4 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots, then adopt the Mo-Si-C alloy cast ingots
Semi-finished product bar is cut into electric spark wire cutting method, the cross-sectional diameter of the bar is 25mm, and length is
850mm；The melting electric current of the electronic torch melting is 4A, and melting voltage is 75kV；
Step 4: semi-finished product bar described in step 3 are carried out with polishing removes surface scale, by described half after polishing
Finished product bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloys are obtained after cooling
Bar；The melting electric current of the electron beam zone melting is 7A, and melting voltage is 60kV.
The shaft-like such as Mo-Si-C alloy bar materials crystal boundary manufactured in the present embodiment is clear-cut, crystal grain is in, without visible fine fisssure
Line and it is empty the defects of, its quality purity is 99.5%, the mass content of impurity oxygen is 40ppm, and room temperature tensile intensity is
1120MPa, Rockwell hardness (HRC) are 60, through 5 × 107Fatigue strength after secondary cycling fatigue experiment is 521MPa, and 1500 DEG C anti-
Tensile strength is 320MPa.
Embodiment 3
The present embodiment Mo-Si-C alloy bar materials are made up of the raw material of following atomic percent：Silicon 15%, carbon 15%, surplus
For molybdenum and inevitable impurity.
The method that the present embodiment prepares Mo-Si-C alloy bar materials comprises the following steps：
It is 200r/ in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
Mim, ratio of grinding media to material are calculated as 5 in mass ratio:Ball milling 20h under conditions of 1, dry after ball milling, mixed under 80 DEG C of vacuum condition
Close powder；The volume of the absolute ethyl alcohol is 1 times of silica flour, carbon dust and molybdenum powder gross mass, and the unit of absolute ethyl alcohol volume is mL,
The unit of silica flour, carbon dust and molybdenum powder gross mass is g；The quality purity of the silica flour is not less than 99.5%, the quality of the carbon dust
Purity is not less than 99.5%, and the quality purity of the molybdenum powder is not less than 99.5%；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering
In stove, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sinterings is obtained after furnace cooling
Body；The temperature of the sintering processes is 2000 DEG C, and time 1h, the blank is that cross sectional dimensions is 50mm (length) × 50mm
The strip-shaped blank of (width)；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than in vacuum
1×10-3Electronic torch melting 2 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots, then adopt the Mo-Si-C alloy cast ingots
Semi-finished product bar is cut into electric spark wire cutting method, the cross-sectional diameter of the bar is 25mm, and length is
850mm；The melting electric current of the electronic torch melting is 2A, and melting voltage is 35kV；
Step 4: semi-finished product bar described in step 3 are carried out with polishing removes surface scale, by described half after polishing
Finished product bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloys are obtained after cooling
Bar；The melting electric current of the electron beam zone melting is 3A, and melting voltage is 40kV.
The shaft-like such as Mo-Si-C alloy bar materials crystal boundary manufactured in the present embodiment is clear-cut, crystal grain is in, without visible fine fisssure
Line and it is empty the defects of, its quality purity is 99.8%, the mass content of impurity oxygen is 30ppm, and room temperature tensile intensity is
1579MPa, Rockwell hardness (HRC) are 65, through 5 × 107Fatigue strength after secondary cycling fatigue experiment is 612MPa, and 1500 DEG C anti-
Tensile strength is 398MPa.
Embodiment 4
The present embodiment Mo-Si-C alloy bar materials are made up of the raw material of following atomic percent：Silicon 18%, carbon 18%, surplus
For molybdenum and inevitable impurity.
The method that the present embodiment prepares Mo-Si-C alloy bar materials comprises the following steps：
It is 300r/ in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
Mim, ratio of grinding media to material are calculated as 10 in mass ratio:Ball milling 30h under conditions of 1, dry after ball milling, mixed under 80 DEG C of vacuum condition
Close powder；The volume of the absolute ethyl alcohol is 2 times of silica flour, carbon dust and molybdenum powder gross mass, and the unit of absolute ethyl alcohol volume is mL,
The unit of silica flour, carbon dust and molybdenum powder gross mass is g；The quality purity of the silica flour is not less than 99.5%, the quality of the carbon dust
Purity is not less than 99.5%, and the quality purity of the molybdenum powder is not less than 99.5%；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering
In stove, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sinterings is obtained after furnace cooling
Body；The temperature of the sintering processes is 2200 DEG C, and time 1.5h, the blank is that cross sectional dimensions is 50mm (length) × 50mm
The strip-shaped blank of (width)；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than in vacuum
1×10-3Electronic torch melting 3 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots, then adopt the Mo-Si-C alloy cast ingots
Semi-finished product bar is cut into electric spark wire cutting method, the cross-sectional diameter of the bar is 25mm, and length is
850mm；The melting electric current of the electronic torch melting is 3A, and melting voltage is 55kV；
Step 4: semi-finished product bar described in step 3 are carried out with polishing removes surface scale, by described half after polishing
Finished product bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloys are obtained after cooling
Bar；The melting electric current of the electron beam zone melting is 5A, and melting voltage is 55kV.
The shaft-like such as Mo-Si-C alloy bar materials crystal boundary manufactured in the present embodiment is clear-cut, crystal grain is in, without visible fine fisssure
Line and it is empty the defects of, its quality purity is 99.5%, the mass content of impurity oxygen is 20ppm, and room temperature tensile intensity is
1125MPa, Rockwell hardness (HRC) are 70, through 5 × 107Fatigue strength after secondary cycling fatigue experiment is 675MPa, and 1500 DEG C anti-
Tensile strength is 415MPa.
Embodiment 5
The present embodiment Mo-Si-C alloy bar materials are made up of the raw material of following atomic percent：Silicon 20%, carbon 30%, surplus
For molybdenum and inevitable impurity.
The method that the present embodiment prepares Mo-Si-C alloy bar materials comprises the following steps：
It is 300r/ in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
Mim, ratio of grinding media to material are calculated as 10 in mass ratio:Ball milling 30h under conditions of 1, dry after ball milling, mixed under 80 DEG C of vacuum condition
Close powder；The volume of the absolute ethyl alcohol is 2 times of silica flour, carbon dust and molybdenum powder gross mass, and the unit of absolute ethyl alcohol volume is mL,
The unit of silica flour, carbon dust and molybdenum powder gross mass is g；The quality purity of the silica flour is not less than 99.5%, the quality of the carbon dust
Purity is not less than 99.5%, and the quality purity of the molybdenum powder is not less than 99.5%；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering
In stove, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sinterings is obtained after furnace cooling
Body；The temperature of the sintering processes is 2100 DEG C, and time 1.5h, the blank is that cross sectional dimensions is 50mm (length) × 50mm
The strip-shaped blank of (width)；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than in vacuum
1×10-3Electronic torch melting 3 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots, then adopt the Mo-Si-C alloy cast ingots
Semi-finished product bar is cut into electric spark wire cutting method, the cross-sectional diameter of the bar is 25mm, and length is
850mm；The melting electric current of the electronic torch melting is 3A, and melting voltage is 55kV；
Step 4: semi-finished product bar described in step 3 are carried out with polishing removes surface scale, by described half after polishing
Finished product bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloys are obtained after cooling
Bar；The melting electric current of the electron beam zone melting is 5A, and melting voltage is 55kV.
The shaft-like such as Mo-Si-C alloy bar materials crystal boundary manufactured in the present embodiment is clear-cut, crystal grain is in, without visible fine fisssure
Line and it is empty the defects of, its quality purity is 99.9%, the mass content of impurity oxygen is 40ppm, and room temperature tensile intensity is
1675MPa, Rockwell hardness (HRC) are 60, through 5 × 107Fatigue strength after secondary cycling fatigue experiment is 512MPa, and 1500 DEG C anti-
Tensile strength is 312MPa.
Embodiment 6
The present embodiment Mo-Si-C alloy bar materials are made up of the raw material of following atomic percent：Silicon 20%, carbon 25%, surplus
For molybdenum and inevitable impurity.
The method that the present embodiment prepares Mo-Si-C alloy bar materials comprises the following steps：
It is 300r/ in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
Mim, ratio of grinding media to material are calculated as 10 in mass ratio:Ball milling 30h under conditions of 1, dry after ball milling, mixed under 85 DEG C of vacuum condition
Close powder；The volume of the absolute ethyl alcohol is 2 times of silica flour, carbon dust and molybdenum powder gross mass, and the unit of absolute ethyl alcohol volume is mL,
The unit of silica flour, carbon dust and molybdenum powder gross mass is g；The temperature of the drying is preferably that the quality purity of the silica flour is not less than
99.5%, the quality purity of the carbon dust is not less than 99.5%, and the quality purity of the molybdenum powder is not less than 99.5%；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering
In stove, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sinterings is obtained after furnace cooling
Body；The temperature of the sintering processes is 2300 DEG C, and time 2.5h, the blank is that cross sectional dimensions is 50mm (length) × 50mm
The strip-shaped blank of (width)；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than in vacuum
1×10-3Electronic torch melting 3 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots, then adopt the Mo-Si-C alloy cast ingots
Semi-finished product bar is cut into electric spark wire cutting method, the cross-sectional diameter of the bar is 25mm, and length is
850mm；The melting electric current of the electronic torch melting is 3A, and melting voltage is 55kV；
Step 4: semi-finished product bar described in step 3 are carried out with polishing removes surface scale, by described half after polishing
Finished product bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloys are obtained after cooling
Bar；The melting electric current of the electron beam zone melting is 5A, and melting voltage is 55kV.
The shaft-like such as Mo-Si-C alloy bar materials crystal boundary manufactured in the present embodiment is clear-cut, crystal grain is in, without visible fine fisssure
Line and it is empty the defects of, its quality purity is 99.8%, the mass content of impurity oxygen is 25ppm, and room temperature tensile intensity is
1665MPa, Rockwell hardness (HRC) are 67, through 5 × 107Fatigue strength after secondary cycling fatigue experiment is 632MPa, and 1500 DEG C anti-
Tensile strength is 389MPa.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and the equivalent structure change that technical spirit is made to above example, still fall within skill of the present invention
In the protection domain of art scheme.
Claims (8)
1. a kind of Mo-Si-C alloy bar materials, it is characterised in that be made up of the raw material of following atomic percent：Silicon 15%~25%,
Carbon 15%~35%, surplus are molybdenum and inevitable impurity.
2. according to a kind of Mo-Si-C alloy bar materials described in claim 1, it is characterised in that by the original of following atomic percent
Material is made：Silicon 18%~20%, carbon 18%~30%, surplus are molybdenum and inevitable impurity.
3. according to a kind of Mo-Si-C alloy bar materials described in claim 2, it is characterised in that by the original of following atomic percent
Material is made：Silicon 20%, carbon 25%, surplus are molybdenum and inevitable impurity.
4. a kind of method for preparing the Mo-Si-C alloy bar materials as described in any claim in claims 1 to 3, its feature exist
In this method comprises the following steps：
It is 200r/min in rotating speed using absolute ethyl alcohol as dispersant Step 1: silica flour, carbon dust and molybdenum powder are placed in ball mill
~400r/min, ratio of grinding media to material are (5~15):Ball milling 20h~40h under conditions of 1, dry after ball milling, obtain under vacuum
Mixed-powder；The volume of the absolute ethyl alcohol be silica flour, 1~3 times of carbon dust and molybdenum powder gross mass, the unit of absolute ethyl alcohol volume
For mL, the unit of silica flour, carbon dust and molybdenum powder gross mass is g；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in sintering furnace
In, it is less than 1 × 10 in vacuum-2It is sintered under conditions of Pa, Mo-Si-C alloy sintered compacts is obtained after furnace cooling；
The temperature of the sintering processes is 2000 DEG C~2400 DEG C, and the time is 1h~3h；
Step 3: Mo-Si-C alloy sintered compacts described in step 2 is placed in electron beam furnace, it is less than 1 in vacuum ×
10-3Electronic torch melting 2~4 times under conditions of Pa, obtain Mo-Si-C alloy cast ingots after cooling, then by the Mo-Si-C alloys
Ingot casting is cut into semi-finished product bar；The melting electric current of the electronic torch melting is 2A~4A, melting voltage be 35kV~
75kV；
Step 4: semi-finished product bar described in step 3 are carried out with polishing removes surface scale, by the semi-finished product after polishing
Bar is less than 1 × 10 in vacuum-3Electron beam zone melting is carried out under conditions of Pa, Mo-Si-C alloy bar materials are obtained after cooling；
The melting electric current of the electron beam zone melting is 3A~7A, and melting voltage is 40kV~60kV.
5. in accordance with the method for claim 4, it is characterised in that the quality purity of silica flour described in step 1 is not less than
99.5%, the quality purity of the carbon dust is not less than 99.5%, and the quality purity of the molybdenum powder is not less than 99.5%.
6. in accordance with the method for claim 4, it is characterised in that the temperature of sintering processes described in step 2 be 2100 DEG C~
2300 DEG C, the time is 1.5h~2.5h.
7. in accordance with the method for claim 6, it is characterised in that the temperature of the sintering processes is 2200 DEG C, time 2h.
8. in accordance with the method for claim 4, it is characterised in that the temperature dried described in step 1 is 80 DEG C~90 DEG C.
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| CN110565169A (en) * | 2019-10-28 | 2019-12-13 | 西北有色金属研究院 | Method for cultivating Mo-Nb-W-Zr alloy single crystal seed crystal |
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| US4180399A (en) * | 1976-09-28 | 1979-12-25 | The Foundation: The Research Institute For Special Inorganic Materials | Molybdenum base composite materials reinforced with continuous silicon carbide fibers and a method for producing the same |
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| CN102424928A (en) * | 2011-12-03 | 2012-04-25 | 西北有色金属研究院 | Mo-Si-B-W multi-phase composite material and preparation method thereof |
| CN105908043A (en) * | 2016-04-27 | 2016-08-31 | 西北有色金属研究院 | Mo-ZrB2-SiC-AlN composite material and preparation method thereof |
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| CN102424928A (en) * | 2011-12-03 | 2012-04-25 | 西北有色金属研究院 | Mo-Si-B-W multi-phase composite material and preparation method thereof |
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| CN110565169A (en) * | 2019-10-28 | 2019-12-13 | 西北有色金属研究院 | Method for cultivating Mo-Nb-W-Zr alloy single crystal seed crystal |
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