CN109382419B - The preparation method of Fe-Al intermetallic compound base microlaminate composites - Google Patents
The preparation method of Fe-Al intermetallic compound base microlaminate composites Download PDFInfo
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- CN109382419B CN109382419B CN201811273720.XA CN201811273720A CN109382419B CN 109382419 B CN109382419 B CN 109382419B CN 201811273720 A CN201811273720 A CN 201811273720A CN 109382419 B CN109382419 B CN 109382419B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/02—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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Abstract
A kind of preparation method of Fe-Al intermetallic compound base microlaminate composites, comprising the following steps: (1) prepare the identical iron plate of length and width and aluminium sheet Jing Guo removing surface, heating carries out sofening treatment and surface polishing respectively；(2) iron plate and aluminium sheet are stacked alternately, between two neighboring iron plate, aluminium foil wraps each aluminium sheet；(3) heating furnace is heated to 400 ± 10 DEG C, is put into hot pressing after blank heat preservation；(4) heating furnace is heated to 400~450 DEG C, is put into hot rolling after heating platen heat preservation；(5) multi-pass cold rolling is carried out, stress relief annealing three times is carried out in cold-rolled process；(6) alloying heat treatment is carried out.The present invention uses the technology path of near-net-shape, solves the problems, such as that intermetallic compound is difficult to following process, and process is simple, process is reasonable, of less demanding to operating environment, raw material are cheap, it is easier to realize industrialized production.
Description
Technical field
The invention belongs to field of material technology, in particular to a kind of Fe-Al intermetallic compound base microlaminate composites
Preparation method.
Background technique
It is strong that long-range order, binding force are arranged between Fe-Al intermetallic compound atom, have the spy of metallic bond and covalent bond concurrently
Sign, thus there is some special physics, chemistry and mechanical property；Meanwhile Fe-Al intermetallic compound also show it is higher
Specific strength and medium temperature intensity have unusual yield strength and temperature relation, and its prices of raw materials is cheap, therefore is considered
It is a kind of high temperature structural material between high temperature alloy and ceramics；As high temperature structural material of new generation and stainless
The alternative materials of steel, Fe-Al intermetallic compound have in fields such as aerospace, auto industry, energy conversion and filtration systems
Have broad application prospects.
However, Fe-Al intermetallic compound has the outstanding problems such as brittleness at room temperature, forming property difference more, seriously constrain
The engineering application of this kind of material；Intermetallic compound base laminated composite materials, which also provide for the solution of these problems, new to be had
Imitate thinking；Intermetallic compound base laminated composite materials are the inspirations by clam shell feature in nature and a kind of novel height designed
Warm structural material；Compound base laminated composite materials are to be made using intermetallic compound as matrix with metal between most metals
The brittleness problems of intermetallic compound are solved for interlayer；This biomimetic features design is established on the basis of energy dissipation mechanism
On, principle is to try to reduce dependence of the mechanical property to original crack defect of material；And with general Strengthening and Toughening means
Higher toughness difference is exchanged for the partial intensities of expendable material, and biomimetic features design is phase interaction in epistasis layer with ductile layers
Under, makes the intensity of material and toughness while being improved.
But higher intensity when due to intermetallic compound inductile at room temperature and low fracture resistance and high temperature
With lower creep strength, make it difficult to be applied to by conventional processing technology in the preparation of laminated material；Existing preparation
In the technique of intermetallic compound base microlaminate composites, SHS situ synthesis techniques improve the brittleness of intermetallic compound
And fracture toughness, but the lift height of composite plate and uniformity are bad after rolling, lead to the distribution of intermetallic compound after reaction
It is undesirable.The preparation process of the multistage heat treatment of method hot rolling collocation can successfully prepare intermetallic compound base lamination composite wood
It can not make each constituent element layer that total tune deformation occur when expecting, but reaching micron order lift height, occur breaking without layering and interlayer
The defects of splitting, and the process conditions such as vacuum degree are required very strict.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Fe-Al intermetallic compound base microlaminate composites, In
Iron plate and aluminium sheet stack after by the way of hot pressing, hot rolling and heat treatment, obtain that plate shape is good, layer by improving process flow
Between the high microlaminate composites of bond strength.
The method of the present invention includes the following steps:
1, prepare the identical iron plate of length and width Jing Guo removing surface and aluminium sheet, wherein iron plate with a thickness of 1mm, the thickness of aluminium sheet
Degree is the 1/3~1/4 of iron plate；By iron plate and aluminium sheet, heating carries out sofening treatment respectively in heating furnace, then carries out surface respectively
Polishing；
2, together with being stacked alternately multiple iron plates by surface polishing with aluminium sheet, each aluminium sheet is located at two neighboring iron
Between plate, then whole aluminium sheets and iron plate are wrapped with aluminium foil, obtain blank；The thickness of the blank formed after aforesaid operations
Degree is 7~9mm；
3, heating furnace is heated to 400 ± 10 DEG C, then blank is placed in heating furnace 20~30min of inside holding, then taken out
Hot pressing is carried out, reduction ratio is 20~35%, obtains heating platen；
4, heating furnace is heated to 400~450 DEG C, then heating platen is placed in heating furnace 10~15min of inside holding, then taken
Hot rolling is carried out out, and reduction ratio is 35~40%, obtains hot rolled plate；
5, hot rolled plate is subjected to multi-pass cold rolling under normal temperature conditions, the reduction ratio of cold rolling is 1~10% per pass, when total
Reduction ratio carries out first time stress relief annealing when reaching 50~60%, is gone for the second time when total reduction reaches 70~74%
Stress annealing carries out third time stress relief annealing when total reduction reaches 78~80%, then proceedes to be cold-rolled to thickness 0.4
~0.5mm obtains cold-reduced sheet；
6, cold-reduced sheet is carried out to alloying heat treatment in heating furnace, aluminium is made to complete Integral alloy, wherein heat treatment temperature
600~650 DEG C of degree, the time 4~for 24 hours, Fe-Al intermetallic compound base microlaminate composites are made.
Quality purity >=99.0% of above-mentioned iron plate, aluminium sheet quality purity >=99.0%.
Above-mentioned surface treatment is iron plate and aluminium sheet to be respectively placed in acetone soln, while being cleaned by ultrasonic at least 20min,
It further takes out and cleans removal acetone with ethanol solution, finally air-dry ethanol solution.
In the above method, when iron plate carries out sofening treatment, iron plate is heated to 600 ± 10 DEG C, keeps the temperature 120 ± 10min, with
Furnace is cooled to 500 ± 10 DEG C, is air-cooled to room temperature；When aluminium sheet carries out sofening treatment, aluminium sheet is heated to 450 ± 10 DEG C, heat preservation 180
± 10min cools to 300 ± 10 DEG C with the furnace, is air-cooled to room temperature.
In above-mentioned step 2, when iron plate and aluminium sheet are stacked alternately, total number of plies of iron plate is n-layer, and total number of plies of aluminium sheet is n-
1 layer, wherein n=6.
The annealing temperature of above-mentioned first time stress relief annealing, second of stress relief annealing and third time stress relief annealing is
400 ± 10 DEG C, annealing time is 4~12h, is air-cooled to room temperature.
Above-mentioned Fe-Al intermetallic compound base microlaminate composites are mainly by multilayer iron layer and at least two layers of Fe-Al
Intermetallic compounds layer is constituted, and has a Fe-Al intermetallic compounds layer, Fe-Al intermetallic between two neighboring iron layer
Have a small amount of residual aluminum and field trash in nitride layer, single layer Fe-Al intermetallic compounds layer with a thickness of 10~30 μm.
Tensile strength of the above-mentioned Fe-Al intermetallic compound base microlaminate composites at 600 DEG C of temperature be 80~
100MPa, the high temperature elongation percentage at 600 DEG C of temperature are 22~30%.
Compared with prior art, the good effect for having the advantage that and generating is the present invention:
1. largely solving intermetallic compound using the technology path of near-net-shape and being difficult to following process
Problem, and process is simple, process is reasonable, of less demanding to operating environment, raw material are cheap, it is easier to realize industry
Metaplasia produces；
2. product by with a thickness of 10~30 μm intermetallic compounds layer and micron order iron layer form, compound interface is straight,
Bond strength is high, without layering and the defects of interlayer faults；Each constituent element layer is while reaching micron order thickness, overall deformation association
It adjusts, lift height is uniform, and alloying distribution is ideal.
Detailed description of the invention
Fig. 1 is the metallurgical microscopic of the Fe-Al intermetallic compound base microlaminate composites in the embodiment of the present invention 1；
Fig. 2 is the Fe-Al intermetallic compound base microlaminate composites cross-section morphology in the embodiment of the present invention 1
SEM figure；
Fig. 3 is the metallurgical microscopic of the Fe-Al intermetallic compound base microlaminate composites in the embodiment of the present invention 2；
Fig. 4 is the Fe-Al intermetallic compound base microlaminate composites cross-section morphology in the embodiment of the present invention 2
SEM figure.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
In the embodiment of the present invention when sofening treatment, cooling rate is in 1.5~2 DEG C/min after heat preservation.
The specification of iron plate and aluminium sheet in the embodiment of the present invention are as follows: long 100mm, wide 20mm.
It carries out using double-roll rolling mill when hot rolling in the embodiment of the present invention, four-high mill is used when cold rolling.
Hot pressing is carried out in the embodiment of the present invention uses press machine.
The equipment that observation metallographic structure uses in the embodiment of the present invention is OLYMPUS-DSX500 inversion type optical microscopy.
The electron-microscope scanning equipment used in the embodiment of the present invention is SSX-550 scanning electron microscope.
In the embodiment of the present invention when sofening treatment when heating, stress relief annealing heating and when Alloying Treatment heating use
Equipment be KSL-1100X batch-type furnace.
Before carrying out hot pressing and hot rolling in the embodiment of the present invention, the equipment used is heated as KSL-1100X batch-type furnace.
Quality purity >=99.0% of the iron plate used in the embodiment of the present invention, aluminium sheet quality purity >=99.0%.
Surface treatment in the embodiment of the present invention is that iron plate and aluminium sheet are respectively placed in acetone soln, is cleaned by ultrasonic simultaneously
At least 20min further takes out and cleans removal acetone with ethanol solution, finally air-dries ethanol solution.
When iron plate carries out sofening treatment in the embodiment of the present invention, iron plate is heated to 600 ± 10 DEG C, heat preservation 120 ±
10min cools to 500 ± 10 DEG C with the furnace, is air-cooled to room temperature；When aluminium sheet carries out sofening treatment, aluminium sheet is heated to 450 ± 10
DEG C, 180 ± 10min is kept the temperature, 300 ± 10 DEG C is cooled to the furnace, is air-cooled to room temperature.
Surface polishing of the present invention, which refers to, removes removing oxide layer for iron plate and surface of aluminum plate polishing.
Aluminum foil thickness is ignored in the embodiment of the present invention.
Embodiment 1
Prepare the identical iron plate of length and width Jing Guo removing surface and aluminium sheet, wherein iron plate with a thickness of 1mm, the thickness of aluminium sheet
For 0.27mm；By iron plate and aluminium sheet, heating carries out sofening treatment respectively in heating furnace, then carries out surface polishing respectively；
Together with multiple iron plates by surface polishing are stacked alternately with aluminium sheet, each aluminium sheet is located at two neighboring iron plate
Between, then whole aluminium sheets and iron plate are wrapped with aluminium foil, obtain blank；Wherein total number of plies of iron plate is 6 layers, aluminium sheet
Total number of plies is 5 layers；The blank formed after aforesaid operations with a thickness of 8.2mm；
Heating furnace is heated to 400 ± 10 DEG C, then blank is placed in heating furnace inside holding 20min, it is single to then take out progress
Passage hot pressing, reduction ratio 32% obtain heating platen；
Heating furnace is heated to 450 DEG C, then heating platen is placed in heating furnace inside holding 10min, then takes out carry out single track
Secondary hot rolling, reduction ratio 39% obtain hot rolled plate, thickness 3.4mm；
Secondary hot rolled plate is subjected to multi-pass cold rolling under normal temperature conditions, the reduction ratio of cold rolling is 1~5% per pass；When
Total reduction carries out first time stress relief annealing when reaching 52%, carries out second of destressing when total reduction reaches 72% and moves back
Fire carries out third time stress relief annealing when total reduction reaches 78%, cold rolling is completed when total reduction reaches 86%, obtains
Cold-reduced sheet；Wherein the annealing temperature of first time stress relief annealing, second of stress relief annealing and third time stress relief annealing is
400 ± 10 DEG C, annealing time is distributed as 4h, 6h and 12h, is air-cooled to room temperature；
Cold-reduced sheet is subjected to alloying heat treatment in heating furnace, so that aluminium is completed Integral alloy, wherein heat treatment temperature
600 DEG C, time 12h, Fe-Al intermetallic compound base microlaminate composites are made；
Fe-Al intermetallic compound base microlaminate composites are mainly by multilayer iron layer between at least two layers of Fe-Al metal
Compound layer is constituted, and has a Fe-Al intermetallic compounds layer between two neighboring iron layer, on Fe-Al intermetallic compounds layer
There are a small amount of residual aluminum and field trash, 20 μm of the average thickness of single layer Fe-Al intermetallic compounds layer；Fe-Al intermetallic compound
The overall thickness of base microlaminate composites is 0.48mm；Its metallurgical microscopic is as shown in Figure 1, cross-section morphology is as shown in Figure 2；
Tensile strength of the Fe-Al intermetallic compound base microlaminate composites at 600 DEG C of temperature is 92MPa, in temperature
High temperature elongation percentage when spending 600 DEG C is 24%.
Embodiment 2
With embodiment 1, difference is method:
(1) third time stress relief annealing is carried out when total reduction reaches 79%；
(6) 650 DEG C of heat treatment temperature, the time is for 24 hours；22 μm of the average thickness of single layer Fe-Al intermetallic compounds layer；Fe-
The metallurgical microscopic of Al intermetallic compound base microlaminate composites is as shown in figure 3, cross-section morphology is as shown in Figure 4；In
Tensile strength at 600 DEG C of temperature is 95MPa, and the high temperature elongation percentage at 600 DEG C of temperature is 22%.
Embodiment 3
With embodiment 1, difference is method:
(1) aluminium sheet with a thickness of 0.25mm；
(2) surface treated and the blank sotck thinkness 7.5mm formed after wrapping；
(3) reduction ratio of single pass hot pressing is 23%；
(4) heating platen is placed in 450 DEG C of heating furnace inside holding 15min, the reduction ratio of single pass hot rolling is 38%；Hot rolled plate
Thickness 3.58mm；
(5) reduction ratio of cold rolling is 4~10% per pass, and first time destressing is carried out when total reduction reaches 58% and is moved back
Fire carries out second of stress relief annealing when total reduction reaches 74%, and third time is carried out when total reduction reaches 79% and is gone
Stress annealing completes cold rolling when total reduction reaches 87%；
(6) 630 DEG C of heat treatment temperature, time 16h；19 μm of the average thickness of single layer Fe-Al intermetallic compounds layer；Fe-
The overall thickness of Al intermetallic compound base microlaminate composites is 0.465mm, and the tensile strength at 600 DEG C of temperature is
84MPa, the high temperature elongation percentage at 600 DEG C of temperature are 30%.
Claims (7)
1. a kind of preparation method of Fe-Al intermetallic compound base microlaminate composites, it is characterised in that the following steps are included:
(1) prepare the identical iron plate of length and width Jing Guo removing surface and aluminium sheet, wherein iron plate with a thickness of 1mm, the thickness of aluminium sheet
It is the 1/3 ~ 1/4 of iron plate thickness；By iron plate and aluminium sheet, heating carries out sofening treatment respectively in heating furnace, then carries out surface respectively
Polishing；
(2) together with being stacked alternately multiple iron plates by surface polishing with aluminium sheet, each aluminium sheet is located at two neighboring iron plate
Between, then whole aluminium sheets and iron plate are wrapped with aluminium foil, obtain blank；The thickness of the blank formed after aforesaid operations
For 7 ~ 9mm；
(3) heating furnace is heated to 400 ± 10 DEG C, then blank is placed in heating furnace 20 ~ 30min of inside holding, then take out progress
Hot pressing, reduction ratio are 20 ~ 35%, obtain heating platen；
(4) heating furnace is heated to 400 ~ 450 DEG C, then heating platen is placed in heating furnace 10 ~ 15min of inside holding, then take out into
Row hot rolling, reduction ratio are 35 ~ 40%, obtain hot rolled plate；
(5) hot rolled plate is subjected to multi-pass cold rolling under normal temperature conditions, the reduction ratio of cold rolling is 1 ~ 10% per pass, when under stagnation pressure
Rate carries out first time stress relief annealing when reaching 50 ~ 60%, carries out second of destressing when total reduction reaches 70 ~ 74% and moves back
Fire carries out third time stress relief annealing when total reduction reaches 78 ~ 80%, then proceedes to be cold-rolled to thickness in 0.4 ~ 0.5mm,
Obtain cold-reduced sheet；
(6) cold-reduced sheet is carried out to alloying heat treatment in heating furnace, so that aluminium is completed Integral alloy, wherein heat treatment temperature
600 ~ 650 DEG C, the time 4 ~ for 24 hours, Fe-Al intermetallic compound base microlaminate composites are made.
2. the preparation method of Fe-Al intermetallic compound base microlaminate composites according to claim 1, feature exist
In quality purity >=99.0% of the iron plate, aluminium sheet quality purity >=99.0%.
3. the preparation method of Fe-Al intermetallic compound base microlaminate composites according to claim 1, feature exist
When iron plate carries out sofening treatment in step (1), iron plate is heated to 600 ± 10 DEG C, 120 ± 10min is kept the temperature, cools to the furnace
500 ± 10 DEG C, it is air-cooled to room temperature；When aluminium sheet carries out sofening treatment, aluminium sheet is heated to 450 ± 10 DEG C, keeps the temperature 180 ± 10min,
It cools to 300 ± 10 DEG C with the furnace, is air-cooled to room temperature.
4. the preparation method of Fe-Al intermetallic compound base microlaminate composites according to claim 1, feature exist
In step (2), when iron plate and aluminium sheet are stacked alternately, total number of plies of iron plate is n-layer, and total number of plies of aluminium sheet is n-1 layers, wherein n=
6。
5. the preparation method of Fe-Al intermetallic compound base microlaminate composites according to claim 1, feature exist
In the first time stress relief annealing, second of stress relief annealing and third time stress relief annealing annealing temperature be 400 ±
10 DEG C, annealing time is 4 ~ 12h, is air-cooled to room temperature.
6. the preparation method of Fe-Al intermetallic compound base microlaminate composites according to claim 1, feature exist
In the Fe-Al intermetallic compound base microlaminate composites mainly by multilayer iron layer between at least two layers of Fe-Al metal
Compound layer is constituted, and has a Fe-Al intermetallic compounds layer between two neighboring iron layer, on Fe-Al intermetallic compounds layer
Have a small amount of residual aluminum and a field trash, single layer Fe-Al intermetallic compounds layer with a thickness of 10 ~ 30 μm.
7. the preparation method of Fe-Al intermetallic compound base microlaminate composites according to claim 1, feature exist
Tensile strength when the Fe-Al intermetallic compound base microlaminate composites are at 600 DEG C of temperature is 80 ~ 100MPa,
High temperature elongation percentage at 600 DEG C of temperature is 22 ~ 30%.
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| CN112644108B (en) * | 2020-12-02 | 2023-03-31 | 中北大学 | Fe-Al intermetallic compound micro-laminated composite material and preparation method thereof |
| CN112706494B (en) * | 2020-12-02 | 2023-01-10 | 中北大学 | Superplastic forming method for high-nitrogen steel/FeAl intermetallic compound micro-laminated composite material |
| CN113477712B (en) * | 2021-07-30 | 2023-12-05 | 安徽工业大学 | Preparation process of multilayer metal composite belt |
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