CN109201736A - A kind of asynchronous rolling method of high-entropy alloy - Google Patents

A kind of asynchronous rolling method of high-entropy alloy Download PDF

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Publication number
CN109201736A
CN109201736A CN201810960014.6A CN201810960014A CN109201736A CN 109201736 A CN109201736 A CN 109201736A CN 201810960014 A CN201810960014 A CN 201810960014A CN 109201736 A CN109201736 A CN 109201736A
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CN
China
Prior art keywords
entropy alloy
rolling
feconicrmn
asynchronous
entropy
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CN201810960014.6A
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Chinese (zh)
Inventor
韩振华
任伟宁
梁山
张凯
刘逸馨
杨玉林
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西安理工大学
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Priority to CN201810960014.6A priority Critical patent/CN109201736A/en
Publication of CN109201736A publication Critical patent/CN109201736A/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B3/00Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences Rolling of aluminium, copper, zinc or other non-ferrous metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working

Abstract

The invention discloses a kind of asynchronous rolling methods of high-entropy alloy, are specifically implemented according to the following steps: step 1, according to the atomic ratios ingredient such as FeCoNiCrMn high-entropy alloy, preparing high-entropy alloy ingot using vacuum arc melting furnace;Step 2, the FeCoNiCrMn high-entropy alloy ingot of preparation is subjected to asymmetrical rolling;Step 3, by the high-entropy alloy after asymmetrical rolling, heat treatment removal residual stress is carried out, keeps the temperature 1h, water quenching under conditions of 800 DEG C of vacuum furnace.A kind of asynchronous rolling method of high-entropy alloy according to the present invention can improve the mechanical property of high-entropy alloy by rationally controlling up-down rollers speed.

Description

A kind of asynchronous rolling method of high-entropy alloy

Technical field

The invention belongs to materials processing technology fields, and in particular to a kind of asynchronous rolling method of high-entropy alloy.

Background technique

In recent years, it was found that a kind of new alloy is referred to as high-entropy alloy (HEAs), is set forth in the 1990s, high entropy closes For gold generally by five kinds or five kinds or more of host element according to grade atomic ratios or close to a kind of alloy of equal atomic ratios, it is to be based on The 1990s bulk amorphous alloys exploitation in the case where propose.High-entropy alloy, which can crystallize, becomes a kind of single crystalline substance Body structure can also be formed containing there are many different crystal structures.Although high-entropy alloy has multicomponent, what is formed is simple Face-centered cubic, body-centered cubic or the face-centered cubic of structure and body-centred cubic mixing.A kind of explain is exactly that positional entropy is equal to conjunction Total free energy makes five kinds or more elements form stable solid solution state microstructure in gold.It is high due to foreign atom huge number Entropy alloy shows as spreading the effects such as slow and severe lattice distortion, so that high-entropy alloy may have one or more simultaneously Outstanding properties, such as high-intensitive and toughness, high rigidity, wear-resisting, superior anti-temper softening characteristic, corrosion-resistant, resistance to high temperature oxidation, this A little superior performances make high-entropy alloy have wide prospects for commercial application.

Sever Plastic Deformation technology, such as Equal-channel Angular Pressing, accumulation pack rolling, high pressure torsion, asymmetrical rolling are super in preparation It is very effective in terms of fine grained texture, it has been applied to multiple material.Asymmetrical rolling refers to that two work roll surface linear velocities are unequal A kind of milling method, also referred to as Asymmetric Rolling usually has following three kinds of forms: (1) not equal asymmetric of upper and lower roller radius Rolling;(2) Asymmetric Rolling that the upper and lower speed of rolls does not wait;(3) top and bottom rolls do not wait non-right with metal rolled piece coefficient of friction Claim rolling.Since heavy reduction rolling may be implemented in asymmetrical rolling, thus crystal grain mechanism also is refined for deformation induced trans- formation and is provided Advantage.Therefore, asymmetrical rolling advantageously reduces recrystallization temperature, reduces energy consumption, is conducive to the mechanics for improving metal rolled piece Performance, and roll-force is reduced, improve production efficiency.Compared with asymmetrical rolling, belongs to using drastic deformation and refine crystal grain Method, such as channel become axis squeeze, Combined Loading (compression plus torsion) etc., due to the limitation of itself, be only applicable to small ruler The laboratory research of very little workpiece can not carry out large-size workpiece large-scale production.And asymmetrical rolling can refine crystal grain and Close large-size workpiece large-scale production.Therefore, there is very wide actual application prospect.

FeCoNiCrMn high-entropy alloy is found to be a kind of single-phase face-centered cubic (fcc) solid solution.Face-centred cubic structure It is bigger than the atom stacking density of body-centered cubic structure, there is lesser lattice diffusion coefficient, therefore plastic deformation with higher Ability.

Summary of the invention

The object of the present invention is to provide a kind of asynchronous rolling methods of high-entropy alloy, can be improved the conjunction of FeCoNiCrMn high entropy Golden mechanical property.

The technical scheme adopted by the invention is that a kind of asynchronous rolling method of high-entropy alloy, specifically according to the following steps Implement:

Step 1, according to the atomic ratios ingredient such as FeCoNiCrMn high-entropy alloy, high entropy is prepared using vacuum arc melting furnace and is closed Ingot;

Step 2, the FeCoNiCrMn high-entropy alloy ingot of preparation is subjected to asymmetrical rolling;

Step 3, by the high-entropy alloy after asymmetrical rolling, heat treatment removal residual stress is carried out, at 800 DEG C of vacuum furnace Under conditions of keep the temperature 1h, water quenching.

The features of the present invention also characterized in that

Step 1 is specifically implemented according to the following steps:

Step 1.1, iron, cobalt, nickel, chromium and manganese raw material powder are taken, is cleaned by ultrasonic with acetone;Then it uses containing quality point Number is the alcoholic solution of 5% nitric acid to manganese raw material powder pickling;

Step 1.2, by each raw material after cleaning according to equal atomic ratios ingredient, with vacuum arc melting furnace, in argon atmosphere Under, melting at least 5 times, last droplet casting becomes the sheet profile FeCoNiCrMn high-entropy alloy of as cast condition.

In step 2, the topping roll speed of milling train and the proportionate relationship of bottom roll speed are adjusted are as follows: 1:2.

In step 2, the topping roll speed for adjusting milling train is 7.5mm/min, bottom roll speed are as follows: 15mm/min.

In step 2, the drafts of the high-entropy alloy after asymmetrical rolling is 90%-95%.

The beneficial effects of the present invention are: asynchronous rolling method of the present invention is reasonable, simple production process, can effectively improve The bulk strength of FeCoNiCrMn high-entropy alloy improves its mechanical property.The method cast using vacuum melting, is rolled by asynchronous Technique processed can obtain the superior high-entropy alloy of performance, its performance is made to meet the requirement in Practical Project field.Formation can practical work The high-entropy alloy and preparation method thereof of industry application.

Detailed description of the invention

Fig. 1 is the room temperature tensile correlation curve of embodiment 1 and comparative example 1 in the present invention;

Fig. 2 is the microhardness correlation curve of embodiment 1 and comparative example 1 in the present invention.

Specific embodiment

The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.

The present invention provides a kind of asynchronous rolling method of high-entropy alloy, is specifically implemented according to the following steps:

Step 1, according to the atomic ratios ingredient such as FeCoNiCrMn high-entropy alloy, high entropy is prepared using vacuum arc melting furnace and is closed Ingot;

Step 1 is specifically implemented according to the following steps:

Step 1.1, iron, cobalt, nickel, chromium and manganese raw material powder is taken to be carried out to remove the impurity and grease in raw material with acetone Ultrasonic cleaning, prevents the performance of the impurity effect high-entropy alloy in raw material;Then the wine containing mass fraction for 5% nitric acid is used Smart solution is easy to aoxidize to manganese raw material powder pickling, manganese, and manganese, which is easy to volatilize, in fusion process additionally to supplement;

Step 1.2, by each raw material after cleaning according to equal atomic ratios ingredient, with vacuum arc melting furnace, in argon atmosphere Under, melting at least 5 times, last droplet casting becomes the sheet profile FeCoNiCrMn high-entropy alloy of as cast condition.

Step 2, the FeCoNiCrMn high-entropy alloy ingot of preparation is subjected to asymmetrical rolling, it is different using the speed of top and bottom rolls To realize asymmetrical rolling;

In step 2, the topping roll speed of milling train and the proportionate relationship of bottom roll speed are adjusted are as follows: 1:2.

In step 2, the topping roll speed for adjusting milling train is 7.5mm/min, bottom roll speed are as follows: 15mm/min.

In step 2, the drafts of the high-entropy alloy after asymmetrical rolling is 90%-95%.

Step 3, the high-entropy alloy after asymmetrical rolling is enclosed quartz ampoule to be heat-treated, residual stress is removed, in vacuum 1h, water quenching are kept the temperature under conditions of 800 DEG C of heating furnace.

Embodiment 1

Step 1, according to the atomic ratios ingredient such as FeCoNiCrMn high-entropy alloy, high entropy is prepared using vacuum arc melting furnace and is closed Ingot;

Step 1 is specifically implemented according to the following steps:

Step 1.1, iron, cobalt, nickel, chromium and manganese raw material powder is taken to be carried out to remove the impurity and grease in raw material with acetone Ultrasonic cleaning, prevents the performance of the impurity effect high-entropy alloy in raw material;Then the wine containing mass fraction for 5% nitric acid is used For smart solution to manganese raw material powder pickling, manganese is oxidizable, and manganese, which is easy to volatilize, in fusion process additionally to supplement;

Step 1.2, by each raw material after cleaning according to equal atomic ratios ingredient, with vacuum arc melting furnace, in argon atmosphere Under, melting at least 5 times, last droplet casting becomes the sheet profile FeCoNiCrMn high-entropy alloy of as cast condition.

Step 2, the FeCoNiCrMn high-entropy alloy ingot of preparation is subjected to asymmetrical rolling, it is different using the speed of top and bottom rolls To realize asymmetrical rolling;

In step 2, the topping roll speed for adjusting milling train is 7.5mm/min, bottom roll speed are as follows: 15mm/min.

In step 2, the drafts of the high-entropy alloy after asymmetrical rolling is 92%.

Step 3, the high-entropy alloy after asymmetrical rolling is enclosed quartz ampoule to be heat-treated, residual stress is removed, in vacuum 1h, water quenching are kept the temperature under conditions of 800 DEG C of heating furnace.

Comparative example

The step 2 that is distinguished as of this comparative example and embodiment 1, this comparative example is using common rolling, the topping roll speed of milling train And lower roller speed is identical are as follows: 7.5mm/min.

By the FeCoNiCrMn high-entropy alloy that commonly rolls and by the FeCoNiCrMn high-entropy alloy of asymmetrical rolling Microhardness comparison such as Fig. 2, it can be seen that the microhardness of asymmetrical rolling is obviously higher than commonly rolling.It commonly rolls micro- hard Spend mean value HV=210.2, asymmetrical rolling microhardness mean value HV=256.2.

Tensile sample size 40mm × 9mm × 2mm, the FeCoNiCrMn high commonly rolled of FeCoNiCrMn high-entropy alloy The FeCoNiCrMn high-entropy alloy stress strain curve of entropy alloy and asymmetrical rolling is as shown in Figure 1.It can will become apparent from from figure asynchronous The tensile strength 805Mpa of rolling, yield strength 521Mpa, the tensile strength 760Mpa commonly rolled, yield strength 416Mpa, Asymmetrical rolling improves 4% than common rolling elongation percentage simultaneously.

Embodiment 2

Step 1, according to the atomic ratios ingredient such as FeCoNiCrMn high-entropy alloy, high entropy is prepared using vacuum arc melting furnace and is closed Ingot;

Step 1 is specifically implemented according to the following steps:

Step 1.1, iron, cobalt, nickel, chromium and manganese raw material powder is taken to be carried out to remove the impurity and grease in raw material with acetone Ultrasonic cleaning, prevents the performance of the impurity effect high-entropy alloy in raw material;Then the wine containing mass fraction for 5% nitric acid is used For smart solution to manganese raw material powder pickling, manganese is oxidizable, and manganese, which is easy to volatilize, in fusion process additionally to supplement;

Step 1.2, by each raw material after cleaning according to equal atomic ratios ingredient, with vacuum arc melting furnace, in argon atmosphere Under, melting at least 5 times, last droplet casting becomes the sheet profile FeCoNiCrMn high-entropy alloy of as cast condition.

Step 2, the FeCoNiCrMn high-entropy alloy ingot of preparation is subjected to asymmetrical rolling, it is different using the speed of top and bottom rolls To realize asymmetrical rolling;

In step 2, the topping roll speed for adjusting milling train is 7.5mm/min, bottom roll speed are as follows: 15mm/min.

In step 2, the drafts of the high-entropy alloy after asymmetrical rolling (will be with a thickness of 10mm's for 90% FeCoNiCrMn high-entropy alloy is rolled, and plate thickness is 0.8 millimeter to the end for rolling).

Step 3, the high-entropy alloy after asymmetrical rolling is enclosed quartz ampoule to be heat-treated, residual stress is removed, in vacuum 1h, water quenching are kept the temperature under conditions of 800 DEG C of heating furnace.

Embodiment 3

Step 1, according to the atomic ratios ingredient such as FeCoNiCrMn high-entropy alloy, high entropy is prepared using vacuum arc melting furnace and is closed Ingot;

Step 1 is specifically implemented according to the following steps:

Step 1.1, iron, cobalt, nickel, chromium and manganese raw material powder is taken to be carried out to remove the impurity and grease in raw material with acetone Ultrasonic cleaning, prevents the performance of the impurity effect high-entropy alloy in raw material;Then the wine containing mass fraction for 5% nitric acid is used For smart solution to manganese raw material powder pickling, manganese is oxidizable, and manganese, which is easy to volatilize, in fusion process additionally to supplement;

Step 1.2, by each raw material after cleaning according to equal atomic ratios ingredient, with vacuum arc melting furnace, in argon atmosphere Under, melting at least 5 times, last droplet casting becomes the sheet profile FeCoNiCrMn high-entropy alloy of as cast condition.

Step 2, the FeCoNiCrMn high-entropy alloy ingot of preparation is subjected to asymmetrical rolling, it is different using the speed of top and bottom rolls To realize asymmetrical rolling;

In step 2, the topping roll speed for adjusting milling train is 7.5mm/min, bottom roll speed are as follows: 15mm/min.

In step 2, the drafts of the high-entropy alloy after asymmetrical rolling is 95%.

Step 3, the high-entropy alloy after asymmetrical rolling is enclosed quartz ampoule to be heat-treated, residual stress is removed, in vacuum 1h, water quenching are kept the temperature under conditions of 800 DEG C of heating furnace.

Advantages of the present invention:

(1) pass through a kind of high-entropy alloy asynchronous rolling method of the invention, the intensity and synthesis of high-entropy alloy can be improved Mechanical property;After heat treatment, the tensile strength of FeCoNiCrMn high-entropy alloy asymmetrical rolling, yield strength, elongation percentage are all bright It is aobvious to improve;After heat treatment, the microhardness of FeCoNiCrMn high-entropy alloy asymmetrical rolling is obviously improved;

(2) method of the invention is fairly obvious to the raising of FeCoNiCrMn high-entropy alloy mechanical property, and is easy to industry Metaplasia produces.

Claims (5)

1. a kind of asynchronous rolling method of high-entropy alloy, which is characterized in that be specifically implemented according to the following steps:
Step 1, according to the atomic ratios ingredient such as FeCoNiCrMn high-entropy alloy, high-entropy alloy is prepared using vacuum arc melting furnace Ingot;
Step 2, the FeCoNiCrMn high-entropy alloy ingot of preparation is subjected to asymmetrical rolling;
Step 3, by the high-entropy alloy after asymmetrical rolling, heat treatment removal residual stress is carried out, in 800 DEG C of item of vacuum furnace 1h, water quenching are kept the temperature under part.
2. a kind of asynchronous rolling method of high-entropy alloy according to claim 1, which is characterized in that the step 1 is specific It follows the steps below to implement:
Step 1.1, iron, cobalt, nickel, chromium and manganese raw material powder are taken, is cleaned by ultrasonic with acetone;Then it uses and is containing mass fraction The alcoholic solution of 5% nitric acid is to manganese raw material powder pickling;
Step 1.2, it by each raw material after cleaning according to equal atomic ratios ingredient, is melted under an argon atmosphere with vacuum arc melting furnace Refining at least 5 times, last droplet casting become the sheet profile FeCoNiCrMn high-entropy alloy of as cast condition.
3. a kind of asynchronous rolling method of high-entropy alloy according to claim 1, which is characterized in that in step 2, adjusting is rolled The topping roll speed of machine and the proportionate relationship of bottom roll speed are as follows: 1:2.
4. a kind of asynchronous rolling method of high-entropy alloy according to claim 1, which is characterized in that in step 2, adjusting is rolled The topping roll speed of machine is 7.5mm/min, bottom roll speed are as follows: 15mm/min.
5. a kind of asynchronous rolling method of high-entropy alloy according to claim 1, which is characterized in that in step 2, process is different The drafts of high-entropy alloy after step rolling is 90%-95%.
CN201810960014.6A 2018-08-22 2018-08-22 A kind of asynchronous rolling method of high-entropy alloy CN109201736A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110157976A (en) * 2019-06-28 2019-08-23 辽宁石油化工大学 A kind of preparation method of the Fe-6.9%Si strip containing rare earth Nd

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106756407A (en) * 2016-12-07 2017-05-31 徐轶 A kind of CrMnFeCoNiZr high-entropy alloys and preparation method thereof
CN107267842A (en) * 2017-06-26 2017-10-20 北京理工大学 A kind of high-melting-point high-entropy alloy and preparation method thereof
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
CN108004452A (en) * 2017-11-27 2018-05-08 北京理工大学 A kind of CoCrFeNiHfxHigh entropy alloy material and preparation method thereof
CN108179343A (en) * 2017-12-28 2018-06-19 上海交通大学 A kind of preparation method of Ultra-fine Grained high-entropy alloy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106756407A (en) * 2016-12-07 2017-05-31 徐轶 A kind of CrMnFeCoNiZr high-entropy alloys and preparation method thereof
CN107267842A (en) * 2017-06-26 2017-10-20 北京理工大学 A kind of high-melting-point high-entropy alloy and preparation method thereof
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
CN108004452A (en) * 2017-11-27 2018-05-08 北京理工大学 A kind of CoCrFeNiHfxHigh entropy alloy material and preparation method thereof
CN108179343A (en) * 2017-12-28 2018-06-19 上海交通大学 A kind of preparation method of Ultra-fine Grained high-entropy alloy

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110157976A (en) * 2019-06-28 2019-08-23 辽宁石油化工大学 A kind of preparation method of the Fe-6.9%Si strip containing rare earth Nd

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