CN110499444A - A kind of nitrogen strengthens FeCrCoMnNi high-entropy alloy and preparation method thereof - Google Patents
A kind of nitrogen strengthens FeCrCoMnNi high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of high-entropy, and in particular to a kind of nitrogen strengthens FeCrCoMnNi high-entropy alloy and preparation method thereof, includes the following steps: the plate that nitrogen reinforcing FeCrCoMnNi high-entropy alloy is cast into 2mm ~ 8mm thickness；The nitrogen of as cast condition is strengthened into FeCrCoMnNi high-entropy alloy and carries out the processing of surface de-oxidation layer；The shear-deformable process operation of heat-flash is carried out using agitating friction technique；The preparation of FeCrCoMnNi high-entropy alloy progress large area plate or tubing is strengthened to nitrogen using horizontally adjacent processing district lap joint process and surface is modified.The present invention provides a kind of nitrogen and strengthens FeCrCoMnNi high-entropy alloy and preparation method thereof, the high-entropy alloy has the characteristics that homogenization and fine, preparation method not only can fast and effeciently eliminate as cast condition gross segregation problem, moreover it is possible to which so that nitrogen is strengthened high-entropy alloy has ultra fine grain structure and high intensity and big ductility.
Description
Technical field
The invention belongs to technical field of high-entropy, and in particular to a kind of nitrogen strengthens FeCrCoMnNi high-entropy alloy and its system
Preparation Method.
Background technique
The distinctive high entropy effect of high-entropy alloy, slow diffusion effect, severe lattice distortion effect and " cocktail " effect,
It is set to have high-intensitive, high rigidity, good wearability, corrosion resistance, fatigue resistance and excellent low temperature and high-temperature mechanics
Can, broad application prospect is shown in numerous areas.Related high-entropy alloy design, preparation and applied basic research have become
Research hotspot in advanced metal material field.
The typical high-entropy alloy put forward earliest is FeCrCoMnNi alloy, which has stable face-centered cubic crystal
Structure simultaneously has high ductility, but its intensity is lower.For the intensity for further increasing the alloy, it is thus proposed that use carbon
Carry out solution strengthening and precipitation strength.By carbon alloy the intensity of alloy is obtained to improve to a certain extent, but plasticity drops
It is low more obvious.Beneficial effect of the nitrogen in high nitrogen stainless steel has been widely recognized, and the solid solution strengthening effect of nitrogen is wanted
Greater than carbon.Patent of invention (107760963 B of CN) proposes a kind of nitrogenous FeCrCoMnNi alloy and preparation method thereof,
Preparation route is melting-forging-cold rolling-annealing, is finally obtained high-strength tenacity nitrogen and strengthens FeCrCoMnNi alloy.But it sends out
Papers written by postgraduates " the N atom pair FeCrCoMnNi high-entropy alloy knot of tissue of bright patent (107760963 B of CN) inventor guidance
The influence of structure and performance " in it has been found that because there is apparent component segregation in ingot casting, appearance when easily leading to forging or hot rolling
The problem of cracking.This not only limits the thermal deformation fragmentation to FeCrCoMnNi high-entropy alloy ingot casting dendrite, also limits simultaneously
Dynamic recrystallization crystal grain refinement under big strain.According to high temperature (1200 DEG C or more), for a long time (generally requiring 12-24 hours)
Annealing is to eliminate component segregation problem, and not only energy consumption is high, and the period is long and crystallite dimension is coarse.Although cold rolling and annealing are refinement gold
Belong to tissue, improve the common method of intensity, but need to change initial workpiece shape and size, is only applicable to high-entropy alloy thin plate
Preparation.
Summary of the invention
The purpose of the present invention is to provide a kind of nitrogen to strengthen FeCrCoMnNi high-entropy alloy and preparation method thereof, which strengthens
FeCrCoMnNi high-entropy alloy has the characteristics that homogenization and fine, and it is macro that preparation method not only can fast and effeciently eliminate as cast condition
See segregation problems, moreover it is possible to which so that nitrogen is strengthened FeCrCoMnNi high-entropy alloy has ultra fine grain structure and high intensity and big
Ductility.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of nitrogen reinforcing FeCrCoMnNi high-entropy alloy, the nitrogen is strengthened nitrogenous used in FeCrCoMnNi high-entropy alloy
The elemental composition (mass percent) of FeCrCoMnNi high-entropy alloy are as follows: iron (5 ~ 35), manganese (5 ~ 35), cobalt (5 ~ 35), chromium (5 ~
35), nickel (5 ~ 35), nitrogen (0.01 ~ 0.4).
A kind of nitrogen strengthens the preparation method of FeCrCoMnNi high-entropy alloy, which is characterized in that includes the following steps,
1), nitrogen reinforcing FeCrCoMnNi high-entropy alloy is cast into the plate of 2mm ~ 8mm thickness；
2) nitrogen of as cast condition, is strengthened into FeCrCoMnNi high-entropy alloy and carries out the processing of surface de-oxidation layer；
3) the shear-deformable process operation of heat-flash, is carried out using agitating friction technique；
4) FeCrCoMnNi high-entropy alloy, is strengthened to nitrogen using horizontally adjacent processing district lap joint process and carries out large area plate or pipe
The preparation of material and surface are modified.
Technical solution of the present invention further improvement lies in that: in step 1) by nitrogen strengthen FeCrCoMnNi high-entropy alloy carry out
High temperature casting uses method for vacuum smelting.
Technical solution of the present invention further improvement lies in that: in step 2) by nitrogen strengthen FeCrCoMnNi high-entropy alloy carry out
Oxide layer processing uses mechanical grinding method.
Technical solution of the present invention further improvement lies in that: in step 3) to nitrogen strengthen FeCrCoMnNi high-entropy alloy use
Agitating friction technique carries out the shear-deformable process operation of heat-flash, specifically includes,
The diameter of the stirring-head insertion workpiece portion of selection is 4 ~ 8mm, is highly 2 ~ 8mm；The speed of agitator of stirring-head be 600 ~
800 turns/min, travel speed is 20 ~ 50mm/min, and inclination angle is 2.5 °；The diameter of the stirring-head rear shaft shoulder is 10 ~ 20mm.
By adopting the above-described technical solution, the technological progress achieved by the present invention is:
The present invention provides a kind of nitrogen to strengthen FeCrCoMnNi high-entropy alloy, and discloses its elemental composition, iron (5 ~ 35), manganese (5
~ 35), cobalt (5 ~ 35), chromium (5 ~ 35), nickel (5 ~ 35), nitrogen (0.01 ~ 0.4)；From element composition on ensure that its have homogenization and
The characteristics of fine.
The present invention provides a kind of shear-deformable features of the heat-flash having using mixing yoghurt, and nitrogen reinforcing is rapidly completed
The process of FeCrCoMnNi high-entropy alloy microstructure homogenization and refinement, saving high temperature long term annealing process and microstructure segregation causes
Problem of Cracking, significantly shorten the processing flow of microstructure homogenization and refinement.Meanwhile strengthening with as cast condition and homogenizing annealing nitrogen
FeCrCoMnNi high-entropy alloy tissue is compared, and the structural homogenity and obdurability after mixing yoghurt are greatly improved.
Nitrogen provided by the invention strengthens the preparation method of FeCrCoMnNi high-entropy alloy, compared with cold rolling and annealing process,
Easily prepared agglomerate body nitrogen strengthens FeCrCoMnNi high-entropy alloy, does not change the original-shape of workpiece in process；With hot rolling
It is compared with forging technology, there is no problem of Cracking when processing for the processing method, can quickly and effectively eliminate the reinforcing of as cast condition nitrogen
FeCrCoMnNi high-entropy alloy dendritic segregation, microstructure homogenization degree are high.
The nitrogen that nitrogen provided by the invention strengthens the preparation method preparation of FeCrCoMnNi high-entropy alloy strengthens FeCrCoMnNi
High-entropy alloy has ultra-fine grain structure, and has high intensity and big ductility.
The preparation method that nitrogen provided by the invention strengthens FeCrCoMnNi high-entropy alloy is environmentally protective, processing cost is low, fits
Strengthen the surface modification and block materials preparation of FeCrCoMnNi high-entropy alloy for nitrogen.It is also applied for other polynary high entropys simultaneously
The microstructure homogenization of alloy and refinement.
Detailed description of the invention
Fig. 1 is the method flow diagram for the preparation method that a kind of nitrogen provided by the invention strengthens FeCrCoMnNi high-entropy alloy；
Fig. 2 is the constituent analysis figure that as cast condition nitrogen strengthens FeCrCoMnNi high-entropy alloy under original process；
Fig. 3 is the nitrogen reinforcing for utilizing a kind of nitrogen provided by the invention to strengthen after the preparation method processing of FeCrCoMnNi high-entropy alloy
FeCrCoMnNi high-entropy alloy constituent analysis figure；
Fig. 4 is that original process and the preparation method for utilizing a kind of nitrogen provided by the invention to strengthen FeCrCoMnNi high-entropy alloy process nitrogen
Strengthen FeCrCoMnNi high-entropy alloy crystallite dimension Statistical Comparison figure；
Fig. 5 is the tensile property that nitrogen strengthens FeCrCoMnNi high-entropy alloy under the various machining states such as original process and present invention process
Comparison diagram.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The present invention provides a kind of nitrogen reinforcing FeCrCoMnNi high-entropy alloy, and the nitrogen strengthens FeCrCoMnNi high-entropy alloy institute
The elemental composition (mass percent) of the nitrogenous FeCrCoMnNi high-entropy alloy used are as follows: iron (5 ~ 35), manganese (5 ~ 35), cobalt (5 ~
35), chromium (5 ~ 35), nickel (5 ~ 35), nitrogen (0.01 ~ 0.4).
The present invention provides a kind of preparation method of nitrogen reinforcing FeCrCoMnNi high-entropy alloy, is generated using mixing yoghurt
Heat-flash it is shear-deformable come fragmentation as cast condition nitrogen strengthen FeCrCoMnNi high-entropy alloy tissue in dendrite, stirred by solid-state machinery
Immixture is segregated to eliminate macro-components；Meanwhile by introducing high density dislocation come further induced chemical homogenization of composition,
Increase dynamic recrystallization nucleation rate and then obtains ultra fine grain tissue.
Further, a kind of nitrogen provided by the invention shown in 1 strengthens the system of FeCrCoMnNi high-entropy alloy with reference to the accompanying drawings
The method flow diagram of Preparation Method, the preparation method that nitrogen provided by the invention strengthens FeCrCoMnNi high-entropy alloy specifically include as follows
Step:
1), nitrogen reinforcing FeCrCoMnNi high-entropy alloy is cast into the plate of 2mm ~ 8mm thickness.
Nitrogen is strengthened into FeCrCoMnNi high-entropy alloy in embodiment provided by the invention and carries out high temperature casting using vacuum
Smelting.
2) nitrogen of as cast condition, is strengthened into FeCrCoMnNi high-entropy alloy and carries out the processing of surface de-oxidation layer.
Nitrogen is strengthened into FeCrCoMnNi high-entropy alloy in embodiment provided by the invention and carries out oxide layer processing using machine
Tool polishing method.
3) the shear-deformable process operation of heat-flash, is carried out using agitating friction technique；
In embodiment provided by the invention, it is highly 2 ~ 8mm that the diameter of the stirring-head insertion workpiece portion of selection, which is 4 ~ 8mm,；
The speed of agitator of stirring-head is 600 ~ 800 turns/min, and travel speed is 20 ~ 50mm/min, and inclination angle is 2.5 °；Stirring-head rear axis
The diameter of shoulder is 10 ~ 20mm.
4) FeCrCoMnNi high-entropy alloy, is strengthened to nitrogen using horizontally adjacent processing district lap joint process and carries out large area plate
Or the preparation and surface modification of tubing.
Specifically, in a specific embodiment provided by the invention, by the casting of one piece of long 200mm, width 100mm, thickness 5mm
State nitrogen strengthens the surface de-oxidation object processing before FeCrCoMnNi high-entropy alloy is processed, and mode is sand paper polishing；Later will
The nitrogen polished strengthens FeCrCoMnNi high-entropy alloy using being rigidly fixed on sample table, then uses shaft shoulder diameter for 15mm
The tungsten-rhenium alloy stirring-head that mixing needle length is 3mm is inserted into workpiece, volume under pressure 3.2mm.Mixing needle with revolving speed is 600rpm, row
It is that 20mm/min is processed into speed.
Further, successively referring under attached original process shown in Fig. 2 as cast condition nitrogen strengthen FeCrCoMnNi high-entropy alloy at
Point analysis chart and attached shown in Fig. 3 added using a kind of preparation method that nitrogen strengthens FeCrCoMnNi high-entropy alloy provided by the invention
Nitrogen after work strengthens FeCrCoMnNi high-entropy alloy constituent analysis figure, and attached original process shown in Fig. 4 and utilization are provided by the invention
A kind of nitrogen strengthens the preparation method processing nitrogen reinforcing FeCrCoMnNi high-entropy alloy crystallite dimension system of FeCrCoMnNi high-entropy alloy
Comparison diagram is counted, nitrogen is strengthened FeCrCoMnNi high entropy and closed under the various machining states such as attached original process shown in fig. 5 and present invention process
The tensile property comparison diagram of gold, can be easy to obtain:
Strengthen FeCrCoMnNi high-entropy alloy than finding with as cast condition nitrogen, nitrogen provided by the invention strengthens FeCrCoMnNi high-entropy alloy
Elemental redistribution uniformity significantly improve, completely eliminate nitrogen strengthen as cast condition high-entropy alloy existing for dendritic segregation.
Specifically, strengthening FeCrCoMnNi alloy to the nitrogen of as cast condition and processing state carries out processing shown in structure observation result
Area is ultrafine-grained (UFG) microstructure, and grain size range is 0.5 to 10 μm, and average grain size is 2.5 μm.Agitating friction adds Qu Qiangdu
832 MPa are reached, fracture elongation has reached 53%, and the tensile property than as cast condition and homogenizing annealing state is significantly increased.
Technical solution disclosed by the invention and the embodiment of offer are to realize that crystal grain refinement obtains height based on large plastometric set
The processing method of intensity and high-elongation, the present invention is not limited to the above embodiments, is joined using the processing for being different from embodiment
Number has good elongation percentage while guaranteeing that nitrogen strengthens FeCrCoMnNi high-entropy alloy with high intensity.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (5)
1. a kind of nitrogen strengthens FeCrCoMnNi high-entropy alloy, which is characterized in that the nitrogen strengthens FeCrCoMnNi high-entropy alloy institute
The elemental composition (mass percent) of the nitrogenous FeCrCoMnNi high-entropy alloy used are as follows: iron (5 ~ 35), manganese (5 ~ 35), cobalt (5 ~
35), chromium (5 ~ 35), nickel (5 ~ 35), nitrogen (0.01 ~ 0.4).
2. the preparation method that a kind of nitrogen strengthens FeCrCoMnNi high-entropy alloy, which is characterized in that include the following steps,
1), nitrogen reinforcing FeCrCoMnNi high-entropy alloy is cast into the plate of 2mm ~ 8mm thickness；
2) nitrogen of as cast condition, is strengthened into FeCrCoMnNi high-entropy alloy and carries out the processing of surface de-oxidation layer；
3) the shear-deformable process operation of heat-flash, is carried out using agitating friction technique；
4) FeCrCoMnNi high-entropy alloy, is strengthened to nitrogen using horizontally adjacent processing district lap joint process and carries out large area plate or pipe
The preparation of material and surface are modified.
3. a kind of nitrogen strengthens the preparation method of FeCrCoMnNi high-entropy alloy according to claim 2, which is characterized in that step
1) nitrogen is strengthened into FeCrCoMnNi high-entropy alloy in and carries out high temperature casting using method for vacuum smelting.
4. a kind of nitrogen strengthens the preparation method of FeCrCoMnNi high-entropy alloy according to claim 2, which is characterized in that step
2) nitrogen is strengthened into FeCrCoMnNi high-entropy alloy in and carries out oxide layer processing using mechanical grinding method.
5. a kind of nitrogen strengthens the preparation method of FeCrCoMnNi high-entropy alloy according to claim 2, which is characterized in that step
3) FeCrCoMnNi high-entropy alloy is strengthened to nitrogen in, the shear-deformable process operation of heat-flash is carried out using agitating friction technique, it is specific to wrap
It includes,
The diameter of the stirring-head insertion workpiece portion of selection is 4 ~ 8mm, is highly 2 ~ 8mm；The speed of agitator of stirring-head be 600 ~
800 turns/min, travel speed is 20 ~ 50mm/min, and inclination angle is 2.5 °；The diameter of the stirring-head rear shaft shoulder is 10 ~ 20mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110860784A (en) * | 2019-12-02 | 2020-03-06 | 东北大学秦皇岛分校 | Friction stir welding method for preparing bulk high-entropy alloy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107760963A (en) * | 2017-10-26 | 2018-03-06 | 福建工程学院 | A kind of nitrogenous FeCoCrNiMn high-entropy alloys and preparation method thereof |
| CN110724949A (en) * | 2019-11-13 | 2020-01-24 | 上海交通大学 | Preparation method of high-entropy alloy layer on surface of medical beta titanium alloy |
-
2019
- 2019-09-04 CN CN201910833535.XA patent/CN110499444A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107760963A (en) * | 2017-10-26 | 2018-03-06 | 福建工程学院 | A kind of nitrogenous FeCoCrNiMn high-entropy alloys and preparation method thereof |
| CN110724949A (en) * | 2019-11-13 | 2020-01-24 | 上海交通大学 | Preparation method of high-entropy alloy layer on surface of medical beta titanium alloy |
Non-Patent Citations (2)
| Title |
|---|
| N. KUMAR等: "Friction Stir Processing of a High Entropy Alloy Al0.1CoCrFeNi", 《THE MINERALS, METALS & MATERIALS SOCIETY》 * |
| 周胜刚等: "《低银含量铅合金电极制备与性能研究》", 31 March 2018 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110860784A (en) * | 2019-12-02 | 2020-03-06 | 东北大学秦皇岛分校 | Friction stir welding method for preparing bulk high-entropy alloy |
| CN110860784B (en) * | 2019-12-02 | 2021-04-13 | 东北大学秦皇岛分校 | Friction stir welding method for preparing bulk high-entropy alloy |
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