CN101219433B - Process for producing intermetallic compound - Google Patents
Process for producing intermetallic compound Download PDFInfo
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- CN101219433B CN101219433B CN2008100101685A CN200810010168A CN101219433B CN 101219433 B CN101219433 B CN 101219433B CN 2008100101685 A CN2008100101685 A CN 2008100101685A CN 200810010168 A CN200810010168 A CN 200810010168A CN 101219433 B CN101219433 B CN 101219433B
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Abstract
The invention relates to a preparation method of intermetallic compound, which is characterized in that iron foil, nickel foil or titanium foil and aluminum foil are adopted as raw materials; the preparation method comprises the steps are that: selecting raw foil material with consideration of the thickness of the raw foil material; defatting, degreasing and surface activation treating; alternative lapping of the treated foil; making rolling blank; warm rolling under heating temperature of 100-180 DEG C and 40-70 percent of rolling draft; edge cutting and cold rolling with 10-20 percent of rolling draft; heat treating of solid-phase alloying under temperature of 400-680 DEG C for 1-5 hours. The invention has the advantages that: the prepared intermetallic compound has uniform fine texture; average grain size is 2-20 Mum; room temperature brittleness and high temperature obdurability of the intermetallic compounds have been greatly improved. The invention overcomes the problem that intermetallic compound is difficult formed and has extensive industrial application value.
Description
Technical field
The present invention relates to a kind of preparation method of intermetallic compound.
Background technology
Among the present existing intermetallic compound preparation method, founding metallurgy method technology is simple, and product cost is low, the production efficiency height, but the material as-cast structure crystal grain that this method obtains is thick, the easy segregation of composition.Powder metallurgy and particle burning synthetic method have been improved the mechanical property of intermetallic compound effectively, but cost is higher, and are difficult to prepare large-scale block, are unsuitable for large-scale industrial production.The molten metal casting forming technique can obtain highly stable Ti-Al intermetallic compound, and its shortcoming is that there is tangible anisotropy in the intermetallic compound for preparing.Rapid solidification method can only prepare the intermetallic compound strip that thickness is 30～50 μ m.SHS original position synthetic technology has been improved the fragility and the fracture toughness of Ni/Al intermetallic compound, but the uniformity of the inter-metallic compound material that this technology obtains is not really desirable, and process conditions such as vacuum is required very strict.
Summary of the invention
The objective of the invention is to overcome the deficiency that existing intermetallic compound technology of preparing exists, provide that a kind of technological process is reasonable, the cycle short; Product properties can be optimized design and effectively control, and the goods specification is complete, is suitable for the preparation method of compound between the industrial-scale production high-performance metal.And can obtain the intermetallic compound plate material with grain refinement feature of large-size, solve the not difficult problem of easy-formation of inter-metallic compound material.
The technical scheme that realizes the object of the invention is: be raw material with the metal foil, undertaken by following processing step:
(1) determines intermetallic compound kind type and shape earlier, select raw material foil composition and thickness;
(2), in cleaning liquid, finish oil removing, grease removal and surface activation process to selected raw material foil;
(3) the raw material foil after the surface treatment is carried out alternately laminated, make rolling blank, rolling sotck thinkness is 3～10mm;
(4) rolling blank is sent into heating furnace, under argon shield, be heated to 100～180 ℃, and be incubated 20～60min; With the roll preheating, the roll surface preheat temperature is identical with blank heating temperature simultaneously; To heat the back blank at last and send into mill milling and become composite plate, rolling reduction ratio is 40～70%;
(5) composite plate behind the warm-rolling is cut edge, carry out cold rolling attenuate then on milling train, cold rolling percentage pass reduction is 10～20%;
(6) cold rolling composite plate is sent into heat-treatment furnace and carried out the heat treatment of solid phase alloying, heat treatment temperature is 400～680 ℃, and heat treatment time is 1～5h.
The metal foil raw material is: iron foil and aluminium foil, nickel foil and aluminium foil or titanium foil and aluminium foil.
Above-mentioned raw materials iron foil, nickel foil, titanium foil and aluminium foil require quality purity all＞99.9%, and raw material thickness is 10～30 μ m.
To the raw material foil, finish oil removing, grease removal and surface activation process in cleaning in the liquid and be: in carbon tetrachloride solution, soaked 5 minutes earlier, in acetone soln, soaked 5 minutes then, after from acetone soln, taking out, in clear water, soaked 5 minutes, afterwards oven dry; Use NaOH solution alkali cleaning 5～15min of 5～10wt% of 30～80 ℃ then, after the clear water flushing of flowing, with the HNO of 20～50 ℃ 20wt%
3Solution pickling 1～5min, air-dry after the clear water flushing of flowing.
It is compound and the composite plate behind the warm-rolling is carried out cold rolling attenuate all select for use four-high mill to be rolled that rolling blank is carried out warm-rolling.
The intermetallic compound composite plate makes composite plate finish whole alloying after Overheating Treatment, and crystallite dimension is 2～20 μ m.
The present invention compared with prior art, the advantage that has and the good effect of generation are:
The present invention is guide with compound between metal target, by raw material foil composition and thickness are selected, the control of rolling technological parameters such as rolling reduction ratio, the adjusting of heat treatment temperature and time, realize the optimal design of inter-metallic compound material, its preparation method advantages of simple, flow process are lacked, are prepared high performance intermetallic compound plate material, have widened the application of intermetallic compound more.
The outstanding feature of the present invention is exactly to have proposed first to make composite plate generation intense plastic strain and obtain the micron order lift height by cold-rolled process.This can make the historrhexis of each interlayer in the composite plate, and crystal grain elongates, to rolling after-baking process median surface forming core, crystallization and the significant effect of grain refinement meeting generation again.
Adopt the intermetallic compound of the present invention's preparation to have uniform micro organization, average grain size is 2～20 μ m, the room temperature fragility of intermetallic compound and high temperature obdurability be improved significantly.The achievement in research of prior art shows, Fe
3Al tensile elongation at room temperature only about 3%, hot strength is lower than 350MPa under 600 ℃ of conditions.And the Fe that adopts this method to prepare
3The Al intermetallic compound since effectively refinement crystal grain (average grain size is 10～15 μ m), eliminated material internal defect simultaneously, the Fe for preparing
3The room temperature tensile percentage elongation of Al intermetallic compound has reached 15～18%, and room temperature tensile strength reaches 720～780MPa, and 600 ℃ of following tensile strength are 480～540MPa.Adopt the Ni of this method preparation
3The room temperature tensile percentage elongation of Al inter-metallic compound material can reach 35～42%, has reached the world level of such material extending performance.Present known Ti
3The room temperature tensile percentage elongation of Al/TiAl synusia shape structural material reaches as high as 2～3%, and the Ti that adopts this method to make
3The intermetallic compound room temperature percentage elongation of Al/TiAll synusia shape structure can reach 3～4%.
The specific embodiment
Embodiment 1: specification is the Fe of 75mm * 10mm * 1.25mm
3The Al intermetallic compound plate material.Adopting Fe content is that 99.98% pure iron foil and aluminium content are that 99.96% pure aluminum foil is a raw material, through the mensuration of the actual lift height of composite plate behind initial raw material foil thickness selection and the warm-rolling, determine that the specification of actual raw material foil is: pure iron foil 15mm * 12mm * 0.027mm; Pure aluminum foil 15mm * 12mm * 0.01mm.Two kinds of raw material foils soaked in carbon tetrachloride solution 5 minutes, and soaked 5 minutes in acetone soln the back, take out the back and soaked 5 minutes in clear water from acetone soln, and oil removing, the grease removal of blank are finished in oven dry afterwards.To the aluminium foil after oil removing, the grease removal, with 30 ℃ 5%NaOH solution alkali cleaning 15min, after the clear water flushing of flowing, with 20 ℃ 20%HNO
3Solution pickling 5min, air-dry after the clear water flushing of flowing, finish the surface active of aluminium foil.Foil after the cleaning is made rolling blank by alternately laminated mode, contains each 200 of two kinds of foils in the blank, and rolling sotck thinkness is 7.4mm.Rolling blank is sent in the 10kW electric furnace and is heated, 100 ℃ of heating-up temperatures, and temperature retention time is 60min, feeds argon gas during heating in stove.Blank heating is right simultaneously
The working roll of four-high mill carries out preheating, and preheat temperature is 100 ℃.Blank after the heating is sent into
It is compound that four-high mill carries out warm-rolling, and rolling reduction ratio is 50%, and composite plate thickness is 3.7mm behind the warm-rolling.The warm-rolling composite plate is sent into after cutting edge
Four-high mill carries out cold rolling attenuate, and the cold rolling pass reduction ratio is 10%, is total to rolling 10 passages, and the thickness of cold rolling back composite plate is 1.25mm.The lift height of iron foil is 2～6 μ m in the cold rolling composite plate, and the lift height of aluminium foil is 1～4 μ m.Composite plate after cold rolling is carried out the heat treatment of whole solid phase alloying in the 15kW electric furnace, heat treatment temperature is 400 ℃, and heat treatment time is 3h.After the whole solid phase Alloying Treatment, composite plate becomes single, uniform Fe through diffusion and phase transformation
3Al intermetallic compound plate material, average grain size are 10～15 μ m.After tested, the Fe that adopts this method to make
3The room temperature percentage elongation of Al intermetallic compound can reach 15～18%, and room temperature tensile strength can reach 720～780MPa, and 600 ℃ of following tensile strength are 480～540MPa.
Embodiment 2: select to the technological process of the cold rolling composite plate that obtains to have Fe/Al synusia shape feature identical with embodiment 1 from raw material foil thickness.The composite plate that different is after cold rolling is carried out the heat treatment of whole solid phase alloying in the 15kW electric furnace, heat treatment temperature is 450 ℃, and heat treatment time is 1h.After the whole solid phase Alloying Treatment, composite plate becomes single, uniform Fe through diffusion and phase transformation
3Al intermetallic compound plate material, average grain size are 12～18 μ m.After tested, the Fe that adopts this method to make
3The room temperature percentage elongation of Al intermetallic compound can reach 13～16%, and room temperature tensile strength can reach 700～750MPa, and 600 ℃ of following tensile strength are 450～500MPa.
Embodiment 3: specification is the Ni of 60mm * 10mm * 1.5mm
3The Al intermetallic compound plate material.Adopting Ni content is that 99.99% pure nickel paper tinsel and aluminium content are that 99.96% pure aluminum foil is a raw material, through the mensuration of the actual lift height of composite plate behind initial raw material foil thickness selection and the warm-rolling, determine that the specification of actual raw material foil is: pure nickel paper tinsel 12mm * 12mm * 0.025mm; Pure aluminum foil 12mm * 12mm * 0.01mm.Two kinds of raw material foils soaked in carbon tetrachloride solution 5 minutes, and soaked 5 minutes in acetone soln the back, take out the back and soaked 5 minutes in clear water from acetone soln, and oil removing, the grease removal of blank are finished in oven dry afterwards.To the aluminium foil after oil removing, the grease removal, with 50 ℃ 10%NaOH solution alkali cleaning 10min, after the clear water flushing of flowing, with 40 ℃ 20%HNO
3Solution pickling 4min, air-dry after the clear water flushing of flowing, finish the surface active of aluminium foil.Foil after the cleaning is made rolling blank by alternately laminated mode, contains each 280 of two kinds of foils in the blank, and rolling sotck thinkness is 9.8mm.Rolling blank is sent in the 10kW electric furnace and is heated, 150 ℃ of heating-up temperatures, and temperature retention time is 30min, feeds argon gas during heating in stove.Blank heating is right simultaneously
The working roll of four-high mill carries out preheating, and preheat temperature is 150 ℃.Blank after the heating is sent into
It is compound that four-high mill carries out warm-rolling, and rolling reduction ratio is 70%, and composite plate thickness is 3mm behind the warm-rolling.The warm-rolling composite plate is sent into after cutting edge
Four-high mill carries out cold rolling attenuate, and the cold rolling pass reduction ratio is 15%, is total to rolling 4 passages, and the thickness of cold rolling back composite plate is 1.5mm.The lift height of nickel foil is 2～5 μ m in the cold rolling composite plate, and the lift height of aluminium foil is 1～4 μ m.Composite plate after cold rolling is carried out the heat treatment of whole solid phase alloying in the 15kW electric furnace, heat treatment temperature is 600 ℃, and heat treatment time is 3h.After the whole solid phase Alloying Treatment, composite plate becomes single, uniform Ni through diffusion and phase transformation
3Al intermetallic compound plate material, average grain size are 5～10 μ m.After tested, the Ni that adopts this method to make
3Al intermetallic compound room temperature percentage elongation can reach 35～42%.
Embodiment 4: select to obtaining to have Ni from raw material foil thickness
/The technological process of the cold rolling composite plate of Al synusia shape feature is identical with embodiment 3.The composite plate that different is after cold rolling is carried out the heat treatment of whole solid phase alloying in the 15kW electric furnace, heat treatment temperature is 550 ℃, and heat treatment time is 5h.After the whole solid phase Alloying Treatment, composite plate becomes single, uniform Ni through diffusion and phase transformation
3Al intermetallic compound plate material, average grain size are 2～8 μ m.After tested, the Ni that adopts this method to make
3Al intermetallic compound room temperature percentage elongation can reach 32～40%.
Embodiment 5: specification is the Ti of 40mm * 10mm * 1.2mm
3The intermetallic compound plate material of Al/TiAl two-phase synusia structure.Adopting Ti content is that 99.95% pure titanium foil and aluminium content are that 99.96% pure aluminum foil is a raw material, through the mensuration of the actual lift height of composite plate behind initial raw material foil thickness selection and the warm-rolling, determine that the specification of actual raw material foil is: pure titanium foil 15mm * 12mm * 0.025mm; Pure aluminum foil 15mm * 12mm * 0.01mm.Two kinds of raw material foils soaked in carbon tetrachloride solution 5 minutes, and soaked 5 minutes in acetone soln the back, take out the back and soaked 5 minutes in clear water from acetone soln, and oil removing, the grease removal of blank are finished in oven dry afterwards.To the aluminium foil after oil removing, the grease removal, air-dry after mobile clear water washes after the clear water flushing of flowing with 80 ℃ 5%NaOH solution alkali cleaning 5min with 50 ℃ 20%HNO3 solution pickling 1min, finish the surface active of aluminium foil.Foil after the cleaning is made rolling blank by alternately laminated mode, contains each 100 of two kinds of foils in the blank, and rolling sotck thinkness is 3.5mm.Rolling blank is sent in the 10kW electric furnace and is heated, 180 ℃ of heating-up temperatures, and temperature retention time is 20min, feeds argon gas during heating in stove.Blank heating is right simultaneously
The working roll of four-high mill carries out preheating, and preheat temperature is 180 ℃.Blank after the heating is sent into
It is compound that four-high mill carries out warm-rolling, and rolling reduction ratio is 40%, and composite plate thickness is 2.1mm behind the warm-rolling.The warm-rolling composite plate is sent into after cutting edge
Four-high mill carries out cold rolling attenuate, and the cold rolling pass reduction ratio is 20%, is total to rolling 3 passages, and the thickness of cold rolling back composite plate is 1.2mm.The lift height of titanium foil is 5～10 μ m in the cold rolling composite plate, and the lift height of aluminium foil is 2～6 μ m.Composite plate after cold rolling is carried out the heat treatment of whole solid phase alloying in the 15kW electric furnace, heat treatment temperature is 620 ℃, and heat treatment time is 4h.After the whole solid phase Alloying Treatment, composite plate becomes with Ti through diffusion and phase transformation
3The Al intermetallic compound is main, contains the synusia shape structure of a small amount of TiAl intermetallic compound, Ti
3The average grain size of Al is 15～18 μ m, and the average grain size of TiAl is 3～6 μ m.After tested, the Ti that adopts this method to make
3Al/TiAl two-phase synusia structural intermetallic compounds room temperature percentage elongation can reach 3～4%.
Embodiment 6: the technological process to the cold rolling composite plate that obtains to have Ti/Al synusia shape feature is identical with embodiment 5.The composite plate that different is after cold rolling is carried out the heat treatment of whole solid phase alloying in the 15kW electric furnace, heat treatment temperature is 680 ℃, and heat treatment time is 2h.After the whole solid phase Alloying Treatment, composite plate becomes with Ti through diffusion and phase transformation
3The Al intermetallic compound is main, contains the synusia shape structure of a small amount of TiAl intermetallic compound, Ti
3The average grain size of Al is 15～20 μ m, and the average grain size of TiAl is 2～5 μ m.After tested, the Ti that adopts this method to make
3Al/TiAl two-phase synusia structural intermetallic compounds room temperature percentage elongation can reach 2～3%.
Claims (4)
1. the preparation method of an intermetallic compound is characterized in that with the metal foil being raw material, is iron foil and aluminium foil, nickel foil and aluminium foil or titanium foil and aluminium foil, and processing step is:
(1) determines intermetallic compound kind type and shape earlier, select raw material foil composition and thickness;
(2) to selected raw material foil, finishing oil removing, grease removal and surface activation process in cleaning liquid is: soaked 5 minutes in carbon tetrachloride solution earlier, soaked 5 minutes in acetone soln then, after taking out from acetone soln, in clear water, soaked 5 minutes, afterwards oven dry; Use NaOH solution alkali cleaning 5～15min of 5～10wt% of 30～80 ℃ then, after the clear water flushing of flowing, with the HNO of 20～50 ℃ 20wt%
3Solution pickling 1～5min, air-dry after the clear water flushing of flowing.
(3) the raw material foil after the surface treatment is carried out alternately laminated, make rolling blank, rolling sotck thinkness is 3～10mm;
(4) rolling blank is sent into heating furnace, under argon shield, be heated to 100～180 ℃, and be incubated 20～60min; With the roll preheating, the roll surface preheat temperature is identical with blank heating temperature simultaneously; To heat the back blank at last and send into mill milling and become composite plate, rolling reduction ratio is 40～70%;
(5) composite plate behind the warm-rolling is cut edge, carry out cold rolling attenuate then on milling train, cold rolling percentage pass reduction is 10～20%;
(6) cold rolling composite plate is sent into heat-treatment furnace and carried out the heat treatment of solid phase alloying, heat treatment temperature is 400～680 ℃, and heat treatment time is 1～5h.
2. according to the preparation method of the described intermetallic compound of claim 1, it is characterized in that requirement raw material iron foil, nickel foil, titanium foil and aluminium foil quality purity all＞99.9%, raw material thickness is 10～30 μ m.
3. according to the preparation method of the described intermetallic compound of claim 1, it is compound and the composite plate behind the warm-rolling is carried out cold rolling attenuate all select for use four-high mill to be rolled to it is characterized in that rolling blank is carried out warm-rolling.
4. according to the preparation method of the described intermetallic compound of claim 1, it is characterized in that the intermetallic compound composite plate makes composite plate finish whole alloying after Overheating Treatment, crystallite dimension is 2～20 μ m.
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Families Citing this family (12)
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| CN101994016B (en) * | 2009-08-12 | 2013-08-14 | 北京航空航天大学 | Titanium-aluminum alloy material and preparation method thereof |
| DE102014009716A1 (en) * | 2014-05-31 | 2015-12-03 | GM Global Technology Operations LLC (n. d. Ges. d. Staates Delaware) | Process for treating sheet metal |
| CN105414219B (en) * | 2015-12-31 | 2018-06-01 | 中国航空工业集团公司北京航空制造工程研究所 | A kind of preparation method of metal/intermetallic compound laminar composite |
| CN107031140A (en) * | 2017-03-29 | 2017-08-11 | 银邦金属复合材料股份有限公司 | The application of composite metal plate containing intermetallic compound |
| CN110142332B (en) * | 2019-05-27 | 2020-07-07 | 大连理工大学 | Forming and property control integrated method for NiAl alloy thin-wall pipe fitting |
| CN110978721B (en) * | 2019-12-18 | 2021-09-10 | 哈尔滨工程大学 | Method for controlling defects and cracking of FeAl intermetallic compound layered composite material |
| CN112183010B (en) * | 2020-09-24 | 2023-01-03 | 桂林电子科技大学 | Design method for reliability of reflow soldering process parameters based on IMC thickness control |
| CN112644108B (en) * | 2020-12-02 | 2023-03-31 | 中北大学 | Fe-Al intermetallic compound micro-laminated composite material and preparation method thereof |
| CN113151701B (en) * | 2021-04-13 | 2022-04-22 | 太原理工大学 | Preparation method of large-size metal aluminide curved surface thin-wall component |
| CN113414238B (en) * | 2021-06-17 | 2022-10-11 | 陕西理工大学 | Molybdenum-nickel-boron metal ceramic material with ultrafine grain oriented distribution and preparation method thereof |
| CN113798394B (en) * | 2021-09-10 | 2022-05-27 | 大连理工大学 | Integrated manufacturing method of high-temperature-resistant thin-wall special-shaped component by laying laminated metal foil strips for blank making |
| CN114480909B (en) * | 2021-12-24 | 2022-11-15 | 北京科技大学 | High-component-uniformity alloy and preparation method thereof |
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