CN101984110B - Preparation method of pre-alloy powder of ferrum-aluminum intermetallic compound Fe2Al5 - Google Patents

Preparation method of pre-alloy powder of ferrum-aluminum intermetallic compound Fe2Al5 Download PDF

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CN101984110B
CN101984110B CN 201010576917 CN201010576917A CN101984110B CN 101984110 B CN101984110 B CN 101984110B CN 201010576917 CN201010576917 CN 201010576917 CN 201010576917 A CN201010576917 A CN 201010576917A CN 101984110 B CN101984110 B CN 101984110B
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powder
iron
intermetallic
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granularity
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CN101984110A (en
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龙坚战
魏修宇
陆必志
方晴
余怀民
李勇
卢少武
管玉明
蒋洪亮
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Zhuzhou Cemented Carbide Group Co Ltd
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Zhuzhou Cemented Carbide Group Co Ltd
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Abstract

The invention discloses a preparation method of pre-alloy powder of a ferrum-aluminum intermetallic compound Fe2Al5 with uniform components and fine granularity, which successively comprises the following steps: proportioning ferrum powder and aluminum powder according to the weight percent of Fe2Al5 and obtaining the uniform mixing powder through ball-milling, mixing and sieving; placing the mixing powder into a container to be flattened; heating the mixing powder to the reaction temperature of the main solid phase of ferrum-aluminum to be sintered at the vacuum or non-oxidative atmosphere; naturally cooling when maintaining the temperature for 4 to 8 hours; and grinding and sieving the obtained Fe2Al5 intermetallic pre-alloy to obtain the pre-alloy powder of the ferrum-aluminum intermetallic compound Fe2Al5. The preparation method of the invention has the advantages of simple technology, high efficiency and low cost.

Description

Iron-Al intermetallic Fe 2Al 5The preparation method of pre-alloyed powder
Technical field
ThisMethod belongs to field of powder metallurgy, relates to a kind of preparation method of pre-alloyed powder of iron-Al intermetallic.
Background technology
The characteristic of metallic bond and covalent linkage coexistence between the long-range order arrangement of intermetallic compound atom and atom, make its use temperature and some mechanical property between Ni based high-temperature alloy and high temperature ceramic material, also has unique superiority at resistance to high temperature oxidation, the aspect such as anticorrosive, such as FeAl, Fe 3The resistance to corrosion of Al intermetallic compound is strong, and weak ferromagnetism is suitable for abominable Working environment.The application direction of Fe-Al series intermetallic compound mainly is the structural part as anti-sulfur-bearing atmosphere and resistance to oxidation atmosphere at present.Fe 3The Al alloy not only has good heat-resisting, wear-resisting and corrosion resistance nature, and its room temperature unit elongation can reach 12.8%, has application potential in various fields such as aviation, chemical industry, nuclear reactor component, smelting furnace high temperature service, electromagnetic components.
Chinese patent (the publication number 101838752A that " utilizes dusty raw materials to make the method for iron aluminum intermetallic compound homogenizing porous material "; open on 09 22nd, 2010 day) a kind of method of utilizing dusty raw materials to make the iron aluminum intermetallic compound homogenizing porous material is disclosed; its key is that the mixed powder to iron powder and aluminium powder has carried out the heat pre-treatment operation before shaping; namely the mixed powder of iron powder and aluminium powder is being heated to 400 ~ 950 ℃ under the anti-oxidation protection atmosphere or under the vacuum; pulverize behind the naturally cooling and mill, its weak point is that its pre-alloyed powder is Fe 2Al 5, FeAl 2, FeAl 3Mixed powder.
Another Chinese patent " is made the method for iron aluminium or Fe-3 Al metal meta-compound elements " (Granted publication CN1061279C, 01 month 31 days calendar year 2001 of the day for announcing), and the method obtains Fe with pure iron and fine aluminium fusing first 2Al 5, FeAl 2, FeAl 3Compound powder adds in proportion straight iron powder again and mixes with above-mentioned powder, and then at normal temperatures compression moulding through liquid phase sintering, can obtain required part, and it adopts intermetallic compound pre-alloyed powder composition is Fe 2Al 5, FeAl 2, FeAl 3Mixture; It adopts the pre-alloyed powder preparation method who atomizes after the melting, and cost is high.
Because the combination reaction between the iron aluminium element powder is a kind of thermopositive reaction, in the combination reaction of fierceness, can discharge a large amount of heats, thereby cause temperature of reaction system to raise rapidly, technological process is uncontrollable, all is to adopt pre-alloyed powder to utilize extruding, HIP(hot isostatic pressing with other element powders so generally adopt powder metallurgy technology to prepare intermetallic compound and matrix material thereof), the technology such as vacuum hotpressing, thermojet make the pre-alloyed powder densification change into intermetallic compound.Required intermetallic compound pre-alloyed powder generally is to adopt the melting obtaining intermetallics, then become pre-alloyed powder by rare gas element or vacuum atomizing, but, adopt the granularity of intermetallic compound pre-alloyed powder of this method preparation thick, in follow-up preparation composite material, in material, form easily " metal pool ", reduced the mechanical property of material.Along with more and more high to the inhomogeneity requirement of the finished product chemical ingredients, it is quite important that the homogeneity of pre-alloyed powder and granularity seem.
Summary of the invention
The object of the present invention is to provide the tiny iron of a kind of homogeneous chemical composition, granularity-Al intermetallic Fe 2Al 5The manufacture method of pre-alloyed powder, and technique is simple, efficient and cost is low.
Iron of the present invention-Al intermetallic Fe 2Al 5The preparation method of pre-alloyed powder, may further comprise the steps successively:
(1) iron powder and aluminium powder are pressed Fe 2Al 5Mass percent batching, ball milling mixes, sieves, and obtains uniform mixed powder; Described iron powder is carbonyl iron dust, granularity 10 μ m-60 μ m; Aluminium powder is the analytical pure aluminium powder, granularity 50 μ m-100 μ m;
(2) place container to pave above-mentioned mixed powder, under vacuum or non-oxidizing atmosphere, be heated to main iron-aluminium solid state reaction temperature and be 550 ℃-640 ℃ and carry out sintering, be incubated 4-8 hour, then naturally cooling obtains Fe 2Al 5The intermetallic prealloy;
(3) with Fe 2Al 5The intermetallic prealloy is milled, is sieved, and obtains iron-Al intermetallic Fe 2Al 5Pre-alloyed powder.
Described heating comprises from room temperature to 400 ℃-450 ℃, heats up to two stages of main solid state reaction temperature, and wherein previous stage, heat-up rate was 3 ℃/min-10 ℃/min, the latter half heat-up rate≤2 ℃/min.
Described Fe 2Al 5Intermetallic pre-alloyed powder granularity is≤40 μ m.
As improvement, described container is cast iron vessel, and mixed powder places the thickness≤10mm that paves of container.
Because Fe 2Al 5Thermomechanical property stable, in iron-aluminium solid state reaction process, generate easily Fe 2Al 5, this intermetallic compound fragility is large simultaneously, and the fragmentation of milling easily can access the little pre-alloyed powder of fine size.Preparation method of the present invention makes and fulfils the heat reaction process between iron powder and aluminium powder ahead of schedule, can reduce the hole that produces owing to diffusion in the follow-up preparation inter-metallic compound material process, add and adopt active strong carbonyl iron dust and analytically pure aluminium powder, thereby further guaranteed homogeneous chemical composition and the mechanical property of alloy material.
As further improvement, so the present invention has adopted the cast iron vessel of good heat conductivity.This is because iron aluminium solid state reaction obtaining intermetallics belongs to thermopositive reaction, the heat of reaction can impel the temperature of powder to raise, after temperature surpasses the fusing point of aluminium, after aluminium is melt into liquid, at capillary force and action of gravitation and move, cause the ununiformity of powder composition; And the heat that cast iron vessel produces the solid state reaction of its reaction can pass away rapidly, guarantees that its reaction synthesis temperature is at solid-state temperature.Simultaneously, because the hole between the powder is larger, heat is difficult for conduction, and the laid thickness of powder is no more than 10mm, has avoided the heat of powder inside to put aside and make the solid state reaction temperature above the fusing point of aluminium.
Description of drawings
Fig. 1 is the iron for preparing of the present invention-Al intermetallic Fe 2Al 5The stereoscan photograph of pre-alloyed powder.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
With granularity be 60 μ mCarbonyl iron dust and granularity 100 μ mThe analytical pure aluminium powder press Fe 2Al 5Mass percent batching, ball milling mixes, crosses 100 mesh sieves, obtains uniform mixed powder; Place cast iron vessel to pave the thickness to 10mm above-mentioned mixed powder, under the vacuum of 1 ~ 5Pa, with the speed of 10 ℃/min, be warmed up to 450 ℃ from room temperature, then the speed with 2 ℃/min is heated to 640 ℃, be incubated 4 hours and carry out sintering, then naturally cooling obtains Fe 2Al 5The intermetallic prealloy; With Fe 2Al 5325 mesh sieves are milled, crossed to the intermetallic prealloy, the acquisition granularity≤ 40 μ mIron-Al intermetallic Fe 2Al 5Pre-alloyed powder, its typical metallograph is seen Fig. 1 (following examples with).Can be seen iron---the Al intermetallic Fe that the inventive method obtains by Fig. 1 2Al 5The pre-alloyed powder homogeneous chemical composition.
Embodiment 2
With granularity be 10 μ mIron powder and granularity 50 μ m'sAluminium powder is pressed Fe 2Al 5Mass percent batching, ball milling mixes, crosses 200 mesh sieves, obtains mixed powder; Place cast iron vessel to pave the thickness to 6mm above-mentioned mixed powder, under hydrogen shield, with the speed of 3 ℃/min, be warmed up to 400 ℃ from room temperature; then the speed with 0.5 ℃/min is heated to 550 ℃; be incubated 8 hours and carry out sintering, then naturally cooling obtains Fe 2Al 5The intermetallic prealloy; With Fe 2Al 5500 mesh sieves are milled, crossed to the intermetallic prealloy, the acquisition granularity≤ 25 μ mIron-Al intermetallic Fe 2Al 5Pre-alloyed powder.
Embodiment 3
With granularity be 30 μ mIron powder and granularity 80 μ mThe analytical pure aluminium powder is pressed Fe 2Al 5Mass percent batching, ball milling mixes, crosses 100 mesh sieves, obtains mixed powder; Place cast iron vessel to pave the thickness to 8mm above-mentioned mixed powder, under argon shield, with the speed of 5 ℃/min, be warmed up to 430 ℃ from room temperature, then the speed with 1 ℃/min is heated to 600 ℃, is incubated 6 hours and carries out sintering, and then naturally cooling obtains Fe 2Al 5The intermetallic prealloy; With Fe 2Al 5425 mesh sieves are milled, crossed to the intermetallic prealloy, obtains granularity≤33 μ mIron-Al intermetallic Fe 2Al 5Pre-alloyed powder.
Embodiment 4
Be that carbonyl iron dust and the granularity of 40 μ m is that 70 μ m aluminium powders are by Fe with granularity 2Al 5Mass percent batching, ball milling mixes, crosses 100 eye mesh screens, obtains mixed powder; Place cast iron vessel to pave the thickness to 8mm above-mentioned mixed powder, under the protection of nitrogen, with the speed of 5 ℃/min, be warmed up to 430 ℃ from room temperature, then the speed with 1 ℃/min is heated to 600 ℃ of temperature, is incubated 6 hours and carries out sintering, and then cooling obtains Fe 2Al 5The intermetallic prealloy; With Fe 2Al 5425 eye mesh screens are milled, crossed to the intermetallic prealloy, the iron of acquisition granularity≤33 μ m-Al intermetallic Fe 2Al 5Pre-alloyed powder.
The iron of the present invention's preparation-Al intermetallic Fe 2Al 5The pre-alloyed powder homogeneous chemical composition, granularity≤ 40 μ m, and technique is simple, efficient is high, cost is low.

Claims (4)

1. iron-Al intermetallic Fe 2Al 5The preparation method of pre-alloyed powder, it is characterized in that the method may further comprise the steps successively: (1) presses Fe with iron powder and aluminium powder 2Al 5Mass percent batching, ball milling mixes, sieves, and obtains uniform mixed powder; Described iron powder is carbonyl iron dust, granularity 10 μ m-60 μ m; Aluminium powder is the analytical pure aluminium powder, granularity 50 μ m-100 μ m; (2) place container to pave above-mentioned mixed powder, under vacuum or non-oxidizing atmosphere, be heated to the main solid state reaction temperature of iron-aluminium and be 550 ℃-640 ℃ and carry out sintering, be incubated 4-8 hour, then naturally cooling obtains Fe 2Al 5The intermetallic prealloy; (3) with Fe 2Al 5The intermetallic prealloy is milled, is sieved, and obtains iron-Al intermetallic Fe 2Al 5Pre-alloyed powder.
2. iron as claimed in claim 1-Al intermetallic Fe 2Al 5The preparation method of pre-alloyed powder, it is characterized in that: described heating comprises from room temperature to 400 ℃-450 ℃, heats up to two stages of main solid state reaction temperature, and wherein previous stage, heat-up rate was 3 ℃/min-10 ℃/min, the latter half heat-up rate≤2 ℃/min.
3. iron as claimed in claim 1-Al intermetallic Fe 2Al 5The preparation method of pre-alloyed powder, it is characterized in that: described Fe 2Al 5Intermetallic pre-alloyed powder granularity is≤40 μ m.
4. iron as claimed in claim 1-Al intermetallic Fe 2Al 5The preparation method of pre-alloyed powder, it is characterized in that: described container is cast iron vessel, mixed powder places the thickness≤10mm that paves of container.
CN 201010576917 2010-12-07 2010-12-07 Preparation method of pre-alloy powder of ferrum-aluminum intermetallic compound Fe2Al5 Active CN101984110B (en)

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CN102672190A (en) * 2011-03-11 2012-09-19 北京有色金属研究总院 Preparation method of prealloying powder
CN102140603B (en) * 2011-03-24 2012-12-19 株洲硬质合金集团有限公司 Preparation method of hard alloy using nickel-aluminum intermetallic compound Ni3Al as bonding phase
CN102162058B (en) * 2011-04-07 2012-10-10 株洲硬质合金集团有限公司 Hard alloy taking nickel-aluminum intermetallic compound Ni3Al as binding phase and preparation method thereof
CN102154582B (en) * 2011-05-27 2013-01-30 株洲硬质合金集团有限公司 Preparation method of hard alloy taking nickel-aluminium intermetallic compound Ni3Al as binding phase
CN102383021B (en) * 2011-11-21 2013-02-13 株洲硬质合金集团有限公司 WC-Co hard alloy with binding phase enhanced by Ni3Al and preparation method thereof
CN103396692A (en) * 2013-08-14 2013-11-20 南京航空航天大学 Radar-infrared compatible stealth material and preparation method thereof
CN105886880B (en) * 2016-04-29 2017-07-11 武汉科技大学 A kind of low-carbon ferroaluminium and preparation method thereof
CN106929711A (en) * 2017-03-14 2017-07-07 郭和谦 A kind of preparation method of the ferro-aluminum composite of high rigidity highly corrosion resistant
US11149331B2 (en) * 2019-08-15 2021-10-19 GM Global Technology Operations LLC Aluminum iron alloy having at least two phases

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