CN105624535A - Preparation method for Fe-Al-Mn-Si alloy - Google Patents
Preparation method for Fe-Al-Mn-Si alloy Download PDFInfo
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Abstract
The invention discloses a preparation method for Fe-Al-Mn-Si alloy. The preparation method comprises the steps that a nano-material preparation method, a powder metallurgy process and a compressing and sintering process are utilized comprehensively, and nanoscale Fe-Al-Mn-Si composite powder bodies are prepared through a mechanical grinding method and are squeezed to be in a block shape; and Fe-Al-Mn-Si alloying is achieved under the hydrogen atmosphere in the low temperature range, and the block-shaped Fe-Al-Mn-Si alloy is obtained. Crystal grains of the Fe-Al-Mn-Si alloy prepared through the nanotechnology are refined, fine dispersed phases are distributed more uniformly, and powder oxidation is effectively reduced. The crystal grains of the Fe-Al-Mn-Si alloy obtained through the preparation method is refined obviously, moreover, the strength, the corrosion resistance and other properties of the Fe-Al-Mn-Si alloy are improved greatly, and the cost is reduced.
Description
Technical field
The preparation method that the present invention relates to a kind of high-temperature alloy material, the preparation method particularly relating to a kind of iron-aluminum-manganese silicon alloy, it is applied to powder metallurgical technology.
Background technology
Phase early 1970s Mechanic Alloying Technology is primarily used for preparation dispersion-strengtherning high temperature alloy, and except preparing high temperature alloy, Mechanic Alloying Technology is also extensively used for preparing structural material. Jangg in 1975 et al. proposes the similar approach of " reaction ball milling ", namely by ball milling chemical additive and metal dust together, brings out cryochemistry reaction, generates the dispersed granules being evenly distributed.
Adopting dispersion strengthening copper alloy prepared by Mechanic Alloying Technology to have the mechanical property of excellence, mechanical alloying dispersion copper alloy can substitute dispersion strengthening copper alloy prepared by internal oxidation, is desirable lead frame and electrode material. In recent years, the research of mechanical alloying dispersion-strengtherning titanium alloy, nickel alloy and molybdenum alloy and mechanical alloying spreading strengthening intermetallic compound is increasing, and estimation will have more novel dispersion-strengthened material to come out.
The method of powder metallurgy is in fact long-standing, and the mankind adopt mechanical crushing method to prepare the powder of gold, silver, copper and bronze early stage, as the decorative paint of pottery etc. PM technique can reduce alloying component segregation to greatest extent, eliminate thick, uneven cast sturcture, the non-equilibrium materials of a series of high-performance such as amorphous, crystallite, accurate brilliant, nanocrystalline and supersaturated solid solution can also be prepared, polytype compound can also be realized, give full play to the respective characteristic of each group element material, be the Technology of a kind of low-cost production high-performance metal base and ceramic composite.
Metal generation corrosion is a kind of naturally ubiquitous phenomenon, and it is very huge for corroding the direct losses brought to metal material. Iron-aluminum-manganese silicon alloy is usually used in the enterprising enforcement use of the turbine of turbocharger for locomotive diesel engine, killed steel and heat-treatment furnace, operates, be the critical component of supercharger under high temperature, high speed and exhaust gas corrosion operating mode. Silicon can significantly improve the corrosion resisting property of material in iron-aluminum-manganese alloy, its reason is probably silicon and forms silicon intermetallic compound in ferroalloy, but high-temperature alloy material prepared by the preparation method of existing iron-aluminum-manganese silicon alloy exists more impurity and is mingled with, affecting the corrosion-resistant of material and heat resistance, prepared material is not met by the instructions for use of complex working condition.
Summary of the invention
In order to solve prior art problem, it is an object of the invention to the deficiency overcoming prior art to exist, the preparation method that a kind of Fe-Al-Mn-Si alloy is provided, combine the advantage of nanotechnology, pressed by powder and sintering technology and PM technique, nanoscale Fe-Al-Mn-Si composite granule is prepared by mechanical milling method, this nano-powder is squeezed into bulk, adopts vacuum double tube heating furnace to realize Fe-Al-Mn-Si alloying in a hydrogen atmosphere, obtain Fe-Al-Mn-Si bulk alloy. During sintering, reducibility gas uses the oxidation effectively just reducing powder, reduce the generation of other oxide impurities, the crystal grain of Fe-Al-Mn-Si alloy prepared by utilization nanotechnology is refined, and the corrosion resisting property of Fe-Al-Mn-Si alloy of gained, specific strength and heat resistance are greatly improved simultaneously. The present invention prepare the method for Fe-Al-Mn-Si alloy be a kind of simple to operate, obtain the method that alloy has corrosion resistance height, thermostability is high.
Create purpose for reaching foregoing invention, adopt following technical proposals:
The preparation method of a kind of Fe-Al-Mn-Si alloy, comprises the steps:
A. the preparation of composite nano-powder: adopt mechanical attrition method, experimental raw reduced iron powder, aluminium powder, manganese powder and nano silica fume are put in ball grinder by certain mass ratio after Homogeneous phase mixing preparation of nano composite granule raw material, add ethanol as dispersant, adopt stearic acid as ball-milling medium, it is re-filled with argon after evacuation in tank, then passing through the ball milling of certain time to prepare composite nano-powder serosity, concrete technology parameter is as follows:
The quality proportioning Fe:Al:Mn:Si of composite nano-powder feed components is 65:8:26:1;
The liquid-solid mass ratio of ethanol and composite nano-powder raw material is 85:15;
Ball-milling Time is 15 ~ 25h; Ball-milling Time is preferably 15 ~ 20h;
Rotational speed of ball-mill is 250 ~ 350rpm; Rotational speed of ball-mill is preferably 250 ~ 300rp;
After ball milling terminates, the composite nano-powder serosity prepared after taking out ball milling, it is placed in vacuum drying oven inner drying, and finally prepares nanoscale Fe-Al-Mn-Si composite granule;
B.Fe-Al-Mn-Si alloy molding: by compressing for the nanoscale Fe-Al-Mn-Si composite granule of preparation in described step a, then vacuum double tube heating furnace is adopted, it is sintered in a hydrogen atmosphere, after lowering the temperature again after completing sintering, finally obtain Fe-Al-Mn-Si alloy profile, preferably by block for the nanoscale Fe-Al-Mn-Si composite granule compacting of preparation in described step a, strip or lamellar, its technological parameter is as follows:
Sintering temperature: 700 ~ 1200 DEG C;
Sintered heat insulating time: 4 ~ 7h;
Molding press power: 250 ~ 400MPa;
Falling temperature gradient: furnace cooling;
Hydrogen flowing quantity: 50 ~ 150mL/min.
The present invention compared with prior art, has following apparent prominent substantive distinguishing features and remarkable advantage:
1. the present invention utilizes nano-powder to prepare the process new technique of Fe-Al-Mn-Si alloy, nanoscale Fe-Al-Mn-Si composite granule is squeezed into bulk, realize Fe-Al-Mn-Si alloying in a hydrogen atmosphere in lower temperature range, obtain Fe-Al-Mn-Si bulk alloy;
2. the present invention uses nanotechnology can not only prepare the Fe-Al-Mn-Si alloy of grain refinement, and the corrosion resistance of this alloy, specific strength and thermostability are greatly improved;
3. the present invention uses hydrogen atmosphere can make to generate powder in-situ reducing the alloying of oxide in mechanical mixture process, so effectively prevent the oxidation of product in Fe-Al-Mn-Si alloying process, it is to avoid impurity produces;
4. the present invention uses sintering furnace technology that the temperature of alloying Fe-Al-Mn-Si also can be greatly lowered, thus realizing being greatly reduced the cost of Fe-Al-Mn-Si alloy production.
Detailed description of the invention
Details are as follows for the preferred embodiments of the present invention:
Embodiment one:
In the present embodiment, the preparation method of a kind of Fe-Al-Mn-Si alloy, comprise the steps:
A. the preparation of composite nano-powder: be taken in anhydrous ethanol medium, adding iron powder, aluminium powder, manganese powder and nano silica fume is 65:8:26:1 in mass ratio, the liquid-solid mass ratio adjusting ethanol and composite nano-powder raw material is 85:15, dispensing loads in stainless steel jar mill after completing, with the rotating speed ball milling 15h of 250r/min on high energy ball mill, prepare nanoscale Fe-Al-Mn-Si composite granule serosity, the Fe-Al-Mn-Si composite granule serosity prepared is carried out vacuum drying, prepares nanoscale Fe-Al-Mn-Si composite granule;
B.Fe-Al-Mn-Si alloy molding: the nanoscale Fe-Al-Mn-Si composite granule of preparation in described step a is pressed into bulk, then vacuum double tube sintering heating furnace is adopted, then it is sintered in temperature range under hydrogen atmosphere in sintering furnace, its technological parameter is: temperature is 700 DEG C, temperature retention time is 4h, press power is 250MPa, and falling temperature gradient is that stove is cold. The flow of hydrogen is 120mL/min. After lowering the temperature again after completing sintering, finally obtain Fe-Al-Mn-Si alloy cube matherial.
The Fe-Al-Mn-Si alloy cube matherial of acquisition is carried out performance test and material phase analysis, and laboratory test results is referring to table 1.
Embodiment two:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, the preparation method of Fe-Al-Mn-Si alloy, comprise the steps:
A. the preparation of composite nano-powder: be taken in anhydrous ethanol medium, adding iron powder, aluminium powder, manganese powder and nano silica fume is 65:8:26:1 in mass ratio, the liquid-solid mass ratio adjusting ethanol and composite nano-powder raw material is 85:15, dispensing loads in stainless steel jar mill after completing, with the rotating speed ball milling 15h of 300r/min on high energy ball mill, prepare nanoscale Fe-Al-Mn-Si composite granule serosity, the Fe-Al-Mn-Si composite granule serosity prepared is carried out vacuum drying, prepares nanoscale Fe-Al-Mn-Si composite granule;
B.Fe-Al-Mn-Si alloy molding: the nanoscale Fe-Al-Mn-Si composite granule of preparation in described step a is pressed into bulk, then vacuum double tube sintering heating furnace is adopted, then it is sintered in temperature range under hydrogen atmosphere in sintering furnace, its technological parameter is: temperature is 700 DEG C, temperature retention time is 4h, press power is 250MPa, and falling temperature gradient is that stove is cold. The flow of hydrogen is 120mL/min. After lowering the temperature again after completing sintering, finally obtain Fe-Al-Mn-Si alloy cube matherial.
The Fe-Al-Mn-Si alloy cube matherial of acquisition is carried out performance test and material phase analysis, and laboratory test results is referring to table 1.
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, the preparation method of Fe-Al-Mn-Si alloy, comprise the steps:
A. the preparation of composite nano-powder: be taken in anhydrous ethanol medium, adding iron powder, aluminium powder, manganese powder and nano silica fume is 65:8:26:1 in mass ratio, the liquid-solid mass ratio adjusting ethanol and composite nano-powder raw material is 85:15, dispensing loads in stainless steel jar mill after completing, with the rotating speed ball milling 20h of 300r/min on high energy ball mill, prepare nanoscale Fe-Al-Mn-Si composite granule serosity, the Fe-Al-Mn-Si composite granule serosity prepared is carried out vacuum drying, prepares nanoscale Fe-Al-Mn-Si composite granule;
B.Fe-Al-Mn-Si alloy molding: the nanoscale Fe-Al-Mn-Si composite granule of preparation in described step a is pressed into bulk, then vacuum double tube sintering heating furnace is adopted, then it is sintered in temperature range under hydrogen atmosphere in sintering furnace, its technological parameter is: temperature is 800 DEG C, temperature retention time is 4h, press power is 250MPa, and falling temperature gradient is that stove is cold. The flow of hydrogen is 120mL/min. After lowering the temperature again after completing sintering, finally obtain Fe-Al-Mn-Si alloy cube matherial.
The Fe-Al-Mn-Si alloy cube matherial of acquisition is carried out performance test and material phase analysis, and laboratory test results is referring to table 1.
Embodiment four:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, the preparation method of Fe-Al-Mn-Si alloy, comprise the steps:
A. the preparation of composite nano-powder: be taken in anhydrous ethanol medium, adding iron powder, aluminium powder, manganese powder and nano silica fume is 65:8:26:1 in mass ratio, the liquid-solid mass ratio adjusting ethanol and composite nano-powder raw material is 85:15, dispensing loads in stainless steel jar mill after completing, with the rotating speed ball milling 20h of 300r/min on high energy ball mill, prepare nanoscale Fe-Al-Mn-Si composite granule serosity, the Fe-Al-Mn-Si composite granule serosity prepared is carried out vacuum drying, prepares nanoscale Fe-Al-Mn-Si composite granule;
B.Fe-Al-Mn-Si alloy molding: the nanoscale Fe-Al-Mn-Si composite granule of preparation in described step a is pressed into bulk, then vacuum double tube sintering heating furnace is adopted, then it is sintered in temperature range under hydrogen atmosphere in sintering furnace, its technological parameter is: temperature is 800 DEG C, temperature retention time is 5h, press power is 250MPa, and falling temperature gradient is that stove is cold. The flow of hydrogen is 120mL/min. After lowering the temperature again after completing sintering, finally obtain Fe-Al-Mn-Si alloy cube matherial.
The Fe-Al-Mn-Si alloy cube matherial of acquisition is carried out performance test and material phase analysis, and laboratory test results is referring to table 1.
Embodiment five:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, the present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, the preparation method of Fe-Al-Mn-Si alloy, comprise the steps:
A. the preparation of composite nano-powder: be taken in anhydrous ethanol medium, adding iron powder, aluminium powder, manganese powder and nano silica fume is 65:8:26:1 in mass ratio, the liquid-solid mass ratio adjusting ethanol and composite nano-powder raw material is 85:15, dispensing loads in stainless steel jar mill after completing, with the rotating speed ball milling 20h of 350r/min on high energy ball mill, prepare nanoscale Fe-Al-Mn-Si composite granule serosity, the Fe-Al-Mn-Si composite granule serosity prepared is carried out vacuum drying, prepares nanoscale Fe-Al-Mn-Si composite granule;
B.Fe-Al-Mn-Si alloy molding: the nanoscale Fe-Al-Mn-Si composite granule of preparation in described step a is pressed into bulk, then vacuum double tube sintering heating furnace is adopted, then it is sintered in temperature range under hydrogen atmosphere in sintering furnace, its technological parameter is: temperature is 800 DEG C, temperature retention time is 5h, press power is 350MPa, and falling temperature gradient is that stove is cold. The flow of hydrogen is 120mL/min. After lowering the temperature again after completing sintering, finally obtain Fe-Al-Mn-Si alloy cube matherial.
The Fe-Al-Mn-Si alloy cube matherial of acquisition is carried out performance test and material phase analysis, and laboratory test results is referring to table 1.
Material property experimental analysis:
The Fe-Al-Mn-Si alloy cube matherial prepared in the above-described embodiments is carried out material phase analysis, the performance test results of Fe-Al-Mn-Si alloy is as shown in table 1, the Fe-Al-Mn-Si alloy structure obtained by nano-powder alloying obtains obvious refinement, effectively reduces crackle and the defect of alloy.
The Fe-Al-Mn-Si alloy obtained is carried out electrochemical property test, and the results are shown in Table 1.
Analytical proof by experiment, utilizes Fe-Al-Mn-Si alloy prepared by the above embodiment of the present invention technology, has very strong decay resistance and higher specific strength, and preparation method is simple and low raw-material cost, is suitable for commercial production and application.
The above embodiment of the present invention combines nanotechnology, PM technique and compacting and sintering technology, nanoscale Fe-Al-Mn-Si composite granule is prepared by mechanical milling method, this nano-powder is squeezed into bulk, and realize Fe-Al-Mn-Si alloying in lower temperature range in a hydrogen atmosphere, obtain Fe-Al-Mn-Si bulk alloy. The crystal grain of Fe-Al-Mn-Si alloy prepared by utilization nanotechnology is refined, and tiny disperse phase distribution is also more uniform, and significantly reduces the oxidation of powder. The crystal grain of Fe-Al-Mn-Si alloy prepared by the above embodiment of the present invention is substantially refined, and its intensity, the performance such as anticorrosive are greatly improved, and reduce cost.
Describe the present invention above in conjunction with embodiment; but the invention is not restricted to above-described embodiment; multiple change can also be made according to the purpose of the innovation and creation of the present invention; change, modification, replacement, combination or the simplification made under all spirit according to technical solution of the present invention and principle; all should be the substitute mode of equivalence; as long as meeting the goal of the invention of the present invention; without departing from the know-why of preparation method and the inventive concept of Fe-Al-Mn-Si alloy of the present invention, broadly fall into protection scope of the present invention.
Claims (3)
1. the preparation method of a Fe-Al-Mn-Si alloy, it is characterised in that comprise the steps:
A. the preparation of composite nano-powder: adopt mechanical attrition method, experimental raw reduced iron powder, aluminium powder, manganese powder and nano silica fume are put in ball grinder by certain mass ratio after Homogeneous phase mixing preparation of nano composite granule raw material, add ethanol as dispersant, adopt stearic acid as ball-milling medium, it is re-filled with argon after evacuation in tank, then passing through the ball milling of certain time to prepare composite nano-powder serosity, concrete technology parameter is as follows:
The quality proportioning Fe:Al:Mn:Si of composite nano-powder feed components is 65:8:26:1;
The liquid-solid mass ratio of ethanol and composite nano-powder raw material is 85:15;
Ball-milling Time is 15 ~ 25h;
Rotational speed of ball-mill is 250 ~ 350rpm;
After ball milling terminates, the composite nano-powder serosity prepared after taking out ball milling, it is placed in vacuum drying oven inner drying, and finally prepares nanoscale Fe-Al-Mn-Si composite granule;
B.Fe-Al-Mn-Si alloy molding: by compressing for the nanoscale Fe-Al-Mn-Si composite granule of preparation in described step a, then vacuum double tube heating furnace is adopted, it is sintered in a hydrogen atmosphere, after lowering the temperature again after completing sintering, finally obtaining Fe-Al-Mn-Si alloy profile, its technological parameter is as follows:
Sintering temperature: 700 ~ 1200 DEG C;
Sintered heat insulating time: 4 ~ 7h;
Molding press power: 250 ~ 400MPa;
Falling temperature gradient: furnace cooling;
Hydrogen flowing quantity: 50 ~ 150mL/min.
2. the preparation method of Fe-Al-Mn-Si alloy according to claim 1, it is characterised in that: in described step b, will in described step a, the nanoscale Fe-Al-Mn-Si composite granule compacting of preparation be block, strip or lamellar.
3. the preparation method of Fe-Al-Mn-Si alloy according to claim 1 or claim 2, it is characterised in that: in described step a, Ball-milling Time is 15 ~ 20h, and rotational speed of ball-mill is 250 ~ 300rp.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109518068A (en) * | 2018-11-30 | 2019-03-26 | 湖南上临新材料科技有限公司 | The preparation method of Fe-Al-Mn-Co alloy |
| CN114163240A (en) * | 2021-12-23 | 2022-03-11 | 中南大学 | Efficient preparation method of sulfur halide compound solid electrolyte |
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| CN114163240A (en) * | 2021-12-23 | 2022-03-11 | 中南大学 | Efficient preparation method of sulfur halide compound solid electrolyte |
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