CN111270056A - Method for heat treatment of alloy containing volatile element in saturated steam environment of the element - Google Patents
Method for heat treatment of alloy containing volatile element in saturated steam environment of the element Download PDFInfo
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- CN111270056A CN111270056A CN202010150701.9A CN202010150701A CN111270056A CN 111270056 A CN111270056 A CN 111270056A CN 202010150701 A CN202010150701 A CN 202010150701A CN 111270056 A CN111270056 A CN 111270056A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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Abstract
The invention provides a method for heat treatment of alloy containing volatile elements in saturated steam environment of the elements. When the alloy containing the volatile elements is subjected to heat treatment in a high vacuum environment, the higher the heat treatment temperature is, the more serious the volatilization loss of the volatile elements is. By placing the elemental substance in a heat treatment environment containing the volatile element alloy, when the elemental substance is melted and volatilized, a saturated vapor environment of the element is quickly formed. Meanwhile, volatile elements in a saturated steam environment permeate into the alloy to form dynamic balance with the volatilization of the elements in the alloy, so that the volatilization loss of the volatile elements in the alloy in the heat treatment process is reduced, the solid-phase reaction of the alloy containing the volatile elements in the heat treatment process is promoted, and the high-purity phase is prepared and obtained. The method has simple process and low cost, can avoid the volatilization loss of volatile elements in the heat treatment process of the alloy containing the volatile elements, and is beneficial to preparing the alloy with uniform and stable components and high phase purity.
Description
Technical Field
The invention belongs to the technical field of alloy preparation, and particularly relates to a heat treatment method of an alloy containing a volatile element in a saturated steam environment of the element, which is particularly suitable for heat treatment of the alloy containing the volatile element.
Background
The purpose of heat treatment is to eliminate internal stress in the alloy and improve the organization structure of the alloy, while the alloy containing volatile elements can generate volatilization loss of the volatile elements in the heat treatment process, so that the components in the alloy are not uniform, the solid phase reaction of the alloy in the heat treatment process is reduced, a high-purity phase is difficult to obtain, and the mechanical, thermal, magnetic, electrical and other macroscopic properties of the alloy are further influenced.
From the current research, in order to reduce the volatilization loss of the volatile element in the heat treatment process of the alloy containing the volatile element, a method of carrying out heat treatment on the alloy containing the volatile element in a high vacuum environment is adopted, but the volatile element has the physical characteristic of volatility, and the volatile element still generates volatilization loss of different degrees even if the heat treatment is carried out in the high vacuum environment. Therefore, a method for avoiding the volatilization loss of the volatile element in the heat treatment process of the alloy containing the volatile element is needed.
Disclosure of Invention
The invention aims to solve the technical problem that the volatilization loss of volatile elements occurs in the heat treatment process of the alloy containing the volatile elements at present, the element simple substance is placed in the heat treatment environment of the alloy containing the volatile elements, and when the volatile element simple substance is melted and volatilized, the saturated steam environment of the element is quickly formed. Meanwhile, volatile elements in a saturated steam environment permeate into the alloy to form dynamic balance with the volatilization of the elements in the alloy, so that the volatilization loss of the volatile elements in the alloy in the heat treatment process is reduced, the solid-phase reaction of the alloy containing the volatile elements in the heat treatment process is promoted, and the high-purity phase is prepared and obtained.
In order to solve the technical problem, the invention provides a method for heat treatment of an alloy containing a volatile element in a saturated steam environment of the element.
Preferably, the method for heat treatment of the alloy containing volatile elements in the saturated steam environment of the elements further comprises some or all of the following technical features:
as an improvement of the technical scheme, the specific method for preparing the high-purity alloy phase containing the volatile element after the alloy containing the volatile element is placed in a saturated steam environment of the volatile element for heat treatment is as follows: polishing to remove oxide layers on the surfaces of all block raw materials, weighing and preparing according to the stoichiometric ratio of the target alloy, repeatedly smelting for 3-10 times in a high-purity inert gas environment, placing the volatile element alloy in a saturated steam environment of the volatile element for annealing after smelting, and obtaining a high-purity alloy phase containing the volatile element.
As an improvement of the above technical solution, the volatile element may include: la, Eu, Mg, Mn, Sn, K, Zn, Bi, Ca, Na, Sr, I2S, Se, Te, P, As.
As an improvement of the technical scheme, the saturated vapor environment of the volatile element can be realized by placing a simple substance of the volatile element in the heat treatment environment.
As an improvement of the technical scheme, the volatile element simple substance needs to be prevented from being in direct contact with the alloy ingot.
As an improvement of the technical scheme, in the smelting process, the alloy containing the volatile element is weighed and configured according to the stoichiometric ratio, and the amount of the simple substance of the volatile element in the alloy is enabled to be 1-10 wt% in excess.
When the alloy containing the volatile elements is subjected to heat treatment in a high vacuum environment, the higher the heat treatment temperature is, the more serious the volatilization loss of the volatile elements is. By placing the elemental substance in a heat treatment environment containing the volatile element alloy, when the elemental substance is melted and volatilized, a saturated vapor environment of the element is quickly formed. Meanwhile, volatile elements in a saturated steam environment permeate into the alloy to form dynamic balance with the volatilization of the elements in the alloy, so that the volatilization loss of the volatile elements in the alloy in the heat treatment process is reduced, the solid-phase reaction of the alloy containing the volatile elements in the heat treatment process is promoted, and the high-purity phase is prepared and obtained.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: the invention provides a heat treatment method of an alloy containing volatile elements in a saturated steam environment of the elements. The alloy containing the volatile element is placed in a saturated steam environment of the element for heat treatment, so that the volatilization loss of the volatile element in the alloy in the heat treatment process can be reduced, and the uniformity and stability of the alloy components are ensured. Volatile elements in a saturated steam environment can permeate into the alloy, so that the solid phase reaction of the alloy containing the volatile elements in the heat treatment process is promoted, and the high-purity physical phase alloy is prepared. The method has simple process and low cost, can avoid the volatilization loss of volatile elements in the heat treatment process of the alloy containing the volatile elements, and is beneficial to preparing the alloy with uniform and stable components and high phase purity.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the contents of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below.
FIG. 1 shows LaFe prepared in example 1 and comparative example 1 of the present invention11Co0.8Si1.2XRD pattern of the alloy.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention.
Example 1
Polishing high-purity block raw materials (99.5% of La, 99.99% of Fe, 99.99% of Si and 99.95% of Co) to remove a surface oxide layer and performing LaFe according to a stoichiometric ratio11Co0.8Si1.2And (5) weighing and preparing. In order to compensate for the volatilization of La during the arc melting process, an excess of 5 wt% was added. And (3) putting the prepared simple substance raw materials into a high-vacuum water-cooled copper crucible arc melting furnace, and repeatedly melting for 5 times in a high-purity argon environment to improve the uniformity of alloy components and prepare the required alloy ingot. In the temperature rise process, due to melting and volatilization of the La block, a La saturated vapor environment can be formed in the closed container, and therefore the obtained alloy ingot and the La block are sealed in a high-vacuum quartz tube. And the La block is required to be prevented from being in direct contact with the alloy ingot, so that the La block and the alloy ingot are prevented from being mutually fused in the heat treatment process. Putting the high-vacuum quartz tube filled with the alloy ingot and the La block into a muffle furnace for annealing at 1100 ℃ for 9 days, and finally quenching with ice water to finally obtain the LaFe annealed in the La saturated steam environment11Co0.8Si1.2And (3) alloying.
Comparative example 1
LaFe was prepared by melting in the same manner as in example 111Co0.8Si1.2Alloy, sealing the obtained alloy ingot in a high vacuum quartz tube without adding La blocks in the high vacuum quartz tube, then putting the high vacuum quartz tube into a muffle furnace for annealing, wherein the annealing process is the same as that of the embodiment 1, and finally obtaining the LaFe annealed in the high vacuum environment11Co0.8Si1.2And (3) alloying.
La(Fe,Si)13The phase composition of the base alloy is as follows: main phase of NaZn13Type structure phase (i.e. 1:13 phase), mixed phase La-rich phase and α -Fe phase, wherein the main phase NaZn13The type structure phase is formed by the La-rich phase and the α -Fe phase through peritectic reaction during the annealing process.And La (Fe, Si)13The rare earth element La in the base alloy belongs to volatile elements, and La can be volatilized and lost when the temperature is higher than the volatilization temperature of La in the heat treatment process, so that La (Fe, Si)13The components in the base alloy are not uniform, the content of the La-rich phase is reduced, the peritectic reaction between the La-rich phase and α -Fe phase in the annealing process is influenced, and the NaZn is further caused13The content of the structural phase is reduced.
TABLE 1 calculation of phase content of each sample in XRD pattern by K-value method in the present invention
As shown in fig. 1, LaFe prepared by annealing in a high vacuum environment and annealing in a La saturated vapor environment, respectively11Co0.8Si1.2XRD results of the alloy. As can be seen, the samples prepared by annealing in a high vacuum environment have the main phase LaCo removed13Phase (NaZn)13Type structure phase) still contains very obvious α -Fe mixed phase, and the sample prepared by annealing in La saturated steam environment contains main phase LaCo13Characteristic diffraction peaks of La-rich phase were not detected in the figure because the La-rich phase was less than the detection limit of XRD (-1%). As shown in Table 1, the compositional percentages of each sample phase in XRD pattern were calculated in Jade software using K-value method, it is known from Table 1 that LaCo, the main phase, was present in samples prepared by annealing in La saturated vapor atmosphere13The content of the phase reaches 95.37 percent, the content of α -Fe impurity phase is 4.63 percent, and the main phase LaCo in a sample prepared by annealing in a high vacuum environment13The content of the phase is 81.17%, but the content of α -Fe impurity phase is 18.83%, the comparison shows that LaFe prepared by annealing in La saturated steam environment11Co0.8Si1.2Main phase LaCo in alloy13The phase content is relatively higher.
The method has simple process and low cost, can avoid the volatilization loss of volatile elements in the heat treatment process of the alloy containing the volatile elements, and is beneficial to preparing the alloy with uniform and stable components and high phase purity.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (3)
1. A method for heat treatment of an alloy containing a volatile element in a saturated vapor environment of the element is characterized in that: the alloy containing the volatile element is placed in a saturated steam environment of the volatile element for heat treatment to prepare and obtain a high-purity alloy phase containing the volatile element.
2. The method of claim 1, wherein the heat treatment of the alloy containing volatile elements in a saturated vapor environment of the elements comprises: the volatile element may include: la, Eu, Mg, Mn, Sn, K, Zn, Bi, Ca, Na, Sr, I2S, Se, Te, P, As.
3. The method of claim 1, wherein the heat treatment of the alloy containing volatile elements in a saturated vapor environment of the elements comprises: the saturated vapor environment of the volatile element can be realized by placing simple substances of the volatile element in the heat treatment environment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629255A (en) * | 2009-07-22 | 2010-01-20 | 厦门钨业股份有限公司 | Low-cost high-performance rare-earth-based AB5-type hydrogen storage alloy and preparation method thereof |
| CN101671770A (en) * | 2009-09-15 | 2010-03-17 | 西部金属材料股份有限公司 | Heat treatment method of alloy containing volatile element |
| CN109136799A (en) * | 2018-09-18 | 2019-01-04 | 广东省稀有金属研究所 | A kind of heat treatment method of the volatile metal hydrogen storage alloy containing low melting point and application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629255A (en) * | 2009-07-22 | 2010-01-20 | 厦门钨业股份有限公司 | Low-cost high-performance rare-earth-based AB5-type hydrogen storage alloy and preparation method thereof |
| CN101671770A (en) * | 2009-09-15 | 2010-03-17 | 西部金属材料股份有限公司 | Heat treatment method of alloy containing volatile element |
| CN109136799A (en) * | 2018-09-18 | 2019-01-04 | 广东省稀有金属研究所 | A kind of heat treatment method of the volatile metal hydrogen storage alloy containing low melting point and application |
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