CN109136799A - A kind of heat treatment method of the volatile metal hydrogen storage alloy containing low melting point and application - Google Patents
A kind of heat treatment method of the volatile metal hydrogen storage alloy containing low melting point and application Download PDFInfo
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- CN109136799A CN109136799A CN201811092864.5A CN201811092864A CN109136799A CN 109136799 A CN109136799 A CN 109136799A CN 201811092864 A CN201811092864 A CN 201811092864A CN 109136799 A CN109136799 A CN 109136799A
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- heat treatment
- hydrogen storage
- melting point
- low melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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Abstract
The present invention provides heat treatment method and the application of a kind of volatile metal hydrogen storage alloy containing low melting point, is related to technical field of alloy thermal treatment.A kind of heat treatment method of the volatile metal hydrogen storage alloy containing low melting point, comprising: the volatile metal hydrogen storage alloy of low melting point and compensation will be contained in closed container while being heat-treated.Metal hydrogen storage alloy is heat-treated using closed container, so that system maintains stable saturated vapour pressure in heat treatment process, it is suppressed that related low-melting-point metal continues to volatilize from alloy, to ensure that the stable content of the volatile metal of low melting point in the alloy.Compensation is heat-treated simultaneously with the volatile metal hydrogen storage alloy containing low melting point, compensation volatilizes low-melting-point metal identical with hydrogen bearing alloy and forms saturated vapour pressure, to reduce the volatilization of low-melting-point metal in hydrogen bearing alloy, the content of low-melting-point metal in hydrogen bearing alloy is improved.The heat treatment method is easy to operate, is suitble to industrialized production.
Description
Technical field
The present invention relates to technical field of alloy thermal treatment, and in particular to a kind of volatile metal hydrogen storage alloy containing low melting point
Heat treatment method and application.
Background technique
Magnesium alloy is very widely used in daily life, from various types of vehicles lightweight structure part, aerospace appts,
To the high-capacity nickel-hydrogen battery cathode hydrogen storage material containing magnesium, the figure of its application can be found.But, the melting of magnesium alloy
Preparation and subsequent heat treatment always exist technical difficulty.This is mainly due to the high melts of alloy and heat treated
Cheng Zhong, the low melting point elements such as magnesium easily volatilize at high temperature, not so as to cause alloying component, phase structure produced etc.
Stablize, thus batch production when batch products stability just at insoluble problem.
Currently, in the heat treatment experiment of the hydrogen bearing alloy containing magnesium, production, people often using control temperature, positive pressure heat at
Reason, using the lighter gas such as helium as the methods of protection gas, to reduce the low melting point elements such as magnesium during heat treatment
Volatile quantity.But all above methods, it is only the evaporation rate for slowing down low melting point element, there is no fundamentally develop
Inhibit the technology of low melting point element volatilization out.
Summary of the invention
The purpose of the present invention is to provide a kind of heat treatment methods of volatile metal hydrogen storage alloy containing low melting point, control low
Volatilization of the melting point metals in heat treatment improves alloying component, property to realize the ratio of adjustment low-melting-point metal in the alloy
The stability of energy.The heat treatment method is easy to operate, is suitble to industrialized production.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of heat treatment method of volatile metal hydrogen storage alloy containing low melting point, comprising:
The volatile metal hydrogen storage alloy of low melting point and compensation will be contained in closed container while being heat-treated.
The beneficial effect comprise that
The volatile metal hydrogen storage alloy containing low melting point is heat-treated using closed container, confined space has blocked container
Interior metal vapors is contacted with the lower region of the temperature such as " cold-zone " in heat-treatment furnace, is avoided when metal vapors encounters " cold-zone " and is coagulated
It ties and leads to the metal saturated vapor drops in heat-treatment furnace, so that the low-melting-point metal in hydrogen bearing alloy continues to volatilize, from
And the case where reducing the ratio of low-melting-point metal in hydrogen bearing alloy.Stable metal vapors pressure reduces the volatile metal of low melting point
The driving force of volatilization, it is suppressed that associated metal continues to volatilize from alloy, to ensure that the content of the metal in the alloy is steady
It is fixed.
It is heat-treated simultaneously using compensation and the volatile metal hydrogen storage alloy containing low melting point.During heat treatment,
Compensation (simple metal block) is more prone to produce volatilization phenomenon compared with hydrogen bearing alloy, and low-melting-point metal takes the lead in volatilizing from compensation
Out, formation and the identical volatile metal vapors containing low melting point in hydrogen bearing alloy, form metal in limited closed container
Vapour pressure.The volatilization of low-melting-point metal in hydrogen bearing alloy is reduced, the content of low-melting-point metal in hydrogen bearing alloy is improved.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the structural schematic diagram of closed container in the embodiment of the present invention；
Fig. 2 is to be carried out at different temperatures 4 hours after being heat-treated, metal hydride using three kinds of different heat treatment methods
Each phase proportion in sample；
Fig. 3 be using three kinds of different heat treatment methods, under the conditions of 950 DEG C, after the heat treatment for carrying out different time, metal
Each phase proportion in hydride sample.
Icon: 100- closed container；110- cabinet；120- case lid；130- sealing element；140- hydrogen bearing alloy；150- compensation
Agent.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Heat treatment method to a kind of volatile metal hydrogen storage alloy containing low melting point of the embodiment of the present invention and application below
It is specifically described.
The embodiment of the invention provides the heat treatment methods of the above-mentioned volatile metal hydrogen storage alloy containing low melting point, comprising:
The volatile metal hydrogen storage alloy of low melting point and compensation will be contained in closed container while being heat-treated.
In existing heat treatment process, there is " cold-zone " in heat-treatment furnace, when the metal steam to volatilize from hydrogen bearing alloy
When gas encounters " cold-zone ", it may occur that condense phenomenon and lead to the metal vapors drops in heat-treatment furnace, so that in hydrogen bearing alloy
Low-melting-point metal continue to volatilize, to reduce the ratio of low-melting-point metal in hydrogen bearing alloy, cause the eutectic in hydrogen bearing alloy
The content and phase structure ratio containing the metallic element of point metal are more difficult to control.
Please refer to Fig. 1, the present invention devises closed container 100 in the heat treatment furnace, blocked in container metal vapors with
The contact of " cold-zone " in heat-treatment furnace.Specifically, closed container 100 includes cabinet 110 and the case lid to match with cabinet 110
120, case lid 120 is covered on the opening of cabinet 110.In order to guarantee the air-tightness of closed container 100, cabinet 110 and case lid 120 connect
It meets place and is equipped with sealing element 130.Sealing element 130 can be metal o-ring circle or other accessories with refractory seals function,
The present invention to it without limitation.
When heat treatment, the volatile metal hydrogen storage alloy 140 of low melting point will be contained and compensation 150 is placed in cabinet 110.It closes
Closed box lid 120 is heat-treated under preset temperature and time.Low-melting-point metal is waved from hydrogen bearing alloy 140 and compensation 150
It issues, forms metal steam air pressure in cabinet 110, the metal vapors to volatilize in compensation 150 is dispersed in hydrogen bearing alloy
Around 140, metal steam air pressure is stabilized, it is suppressed that it continues to volatilize from hydrogen bearing alloy 140, ensure that low-melting-point metal exists
Stable content in alloy.
In the present invention, low-melting-point metal includes at least one of Mg, Sm, Nd, Al, Sm, Sn and Zn.Compensation is
Metal product containing corresponding low-melting-point metal, such as low-melting-point metal block.During heat treatment, compensation (simple gold
Belong to block) it is more prone to produce volatilization phenomenon compared with hydrogen bearing alloy, therefore take the lead in low-melting-point metal identical in hydrogen bearing alloy from compensation
In volatilize, in limited closed container formed saturation metal steam air pressure, reduce hydrogen bearing alloy in low-melting-point metal volatilization,
Stabilize the content of low-melting-point metal in hydrogen bearing alloy.Meanwhile stable vapour pressure reduces low-melting-point metal in hydrogen bearing alloy
The driving force of volatilization improves the controllability that low-melting-point metal volatilizees in hydrogen bearing alloy.
By the research of inventor, the content of the low-melting-point metal in compensation and hydrogen bearing alloy is closed with certain proportion
System.The metal evaporated when the mass ratio of low-melting-point metal in compensation and hydrogen bearing alloy is 0.0005~0.5:1, in compensation
Steam actively forms saturated vapour pressure, can preferably limit the volatilization of low-melting-point metal in hydrogen bearing alloy.Wherein, compensation and
The mass ratio of low-melting-point metal in hydrogen bearing alloy can for 0.001:1,0.005:1,0.0008:1,0.007:1,0.01:1,
0.05:1、0.06:1、0.1:1、0.2:1、0.3:1。
Heat treatment method used in the embodiment of the present invention includes: to store up under conditions of 800~1000 DEG C to low-melting-point metal
Hydrogen alloy is heat-treated 2~20h.Wherein, common heat treatment temperature can be 850,900,950 DEG C in production, generally select
Heat treatment time can be 4,6,10 hours.
The heat treatment method of low-melting-point metal hydrogen bearing alloy provided by the invention is easy to operate, and controllability is strong, suitable for containing
The heat treatment of the alloy of the volatile metallic element of low melting point acts on significant, suitable batch chemical industry in terms of the volatilization of control magnesium
Production.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
Present embodiments provide a kind of heat treatment method of volatile metal hydrogen storage alloy containing low melting point, comprising:
Metal hydride sample is taken, magnesium is contained.The metal hydride sample and MAG block are put into closed container simultaneously into
Row heat treatment.Metal hydride sample gross mass 50g, content of magnesium are 1.5% or so, MAG block 0.3g.The temperature of heat treatment is
800 DEG C, heat treatment time is 2 hours.
Embodiment 2~11
Embodiment 2~11 each provides a kind of heat treatment method of volatile metal hydrogen storage alloy containing low melting point, with reality
The difference for applying example 1 is mainly as follows:
1 heat treatment parameter of table
Comparative example 1
This comparative example, which is provided, is heat-treated hydrogen bearing alloy using prior heat treatment method, chooses and 1 phase of embodiment
The same metal hydride sample containing magnesium, puts it into heat-treatment furnace, is heat-treated 2 hours under conditions of 800 DEG C.
Comparative example 2~11
Comparative example 2~11 each provides a kind of heat treatment method of volatile metal hydrogen storage alloy containing low melting point, and right
The difference of ratio 1 is mainly as follows:
2 heat treatment parameter of table
Comparative example 12
This comparative example provides a kind of heat treatment method, comprising: chooses the metal hydride same as Example 1 containing magnesium
Sample is put it into closed container, is heat-treated 2 hours under conditions of 800 DEG C.
Comparative example 13~22
Comparative example 13~22 each provides a kind of heat treatment method of volatile metal hydrogen storage alloy containing low melting point, and right
The difference of ratio 12 is mainly as follows:
3 heat treatment parameter of table
Test example
The metal alloy provided Examples 1 to 4, embodiment 7, embodiment 9~11, comparative example 1~22 detects, and counts
The loss late of the magnesium of different heat treatment technique is calculated, the result is as follows:
The loss late (%) of magnesium after heat treatment in 4 different temperatures of table 2 hours
As shown in Table 4, as the temperature rises and gradually rises for the loss late of magnesium element content in alloy.When temperature is more than
It after 800 DEG C, is influenced by magnesium saturated vapour pressure, the content loss speed of magnesium is accelerated in metal hydride sample.At traditional heat
Under reason mode, magnesium elements loss amount at 1000 DEG C in alloy is close to 12%.The embodiment 9~12 of closed heat treatment is carried out
The loss late of metal hydride sample magnesium elements after 1000 DEG C of heat treatment is 8.9%, and is carried out fully according to mode of the present invention
The loss late of magnesium elements is only 2.3% after 1000 DEG C of metal hydride sample heat treatments of the Examples 1 to 4 of heat treatment.Explanation
The heat treatment method of hydrogen bearing alloy provided by the invention containing low-melting-point metal can inhibit the volatilization of low-melting-point metal, improve alloy
Ingredient.
Table 5 undergoes the loss late (%) of magnesium after different heat treatment time-triggered protocol at 950 DEG C
As shown in Table 5, the metal hydride sample of the comparative example 3,7,9,10 after being heat-treated using prior heat treatment mode
Product, with the increase of heat treatment time, the loss late of Mg element is also continuously increased, and experience was moved back up to 10 hours at 950 DEG C
After fire, the loss late of magnesium is up to 17.2% in sample.In contrast, it is heat-treated using the closed container of the invention patent
The metal hydride sample of comparative example 14,18,20,21 and the embodiment 3 being heat-treated completely by the method for the present invention, 7,9,
The magnesium loss late of 10 metal hydride sample is then much lower, and under the premise of temperature-resistant, magnesium loss will not with heat at
It manages the increase of time and significantly changes.This is obviously because in closed container provided by the invention, in the heat of setting
Stable vapour pressure, the inhibition of stable vapour pressure continuous and effective in prolonged heat treatment process can be formed under treatment temperature
Magnesium elements volatilize outward from alloy.Under prior heat treatment mode, since burner hearth is big, temperature is unbalanced, there are cold-zone influences etc.
Factor cannot achieve the stability contorting of magnesium elements.
Using detection means such as ICP, XRD, analyzes the chemical component of the alloy product of each embodiment and comparative example and mutually tie
Structure, phase composition.With Rietveld calculation method, the analytical calculation of each Phase Proportion has been carried out to each alloy product.As a result such as Fig. 1
And Fig. 2.
Fig. 2 is to be carried out at different temperatures 4 hours after being heat-treated, metal hydride using three kinds of different heat treatment methods
Each phase proportion in sample.Fig. 3 is to carry out the heat of different time under the conditions of 950 DEG C using three kinds of different heat treatment methods
After processing, each phase proportion in metal hydride sample.In Fig. 2 and Fig. 3, I is that prior heat treatment method is used in comparative example
Comparative example, II is the comparative example being heat-treated in comparative example using closed container, and III is to be mentioned in embodiment using the present invention
The embodiment of the heat treatment method of confession.
From the data of Fig. 2 and Fig. 3 it is found that using the metal of the comparative example 16~19,21,22 of obturator of the invention
The metal hydride sample of hydride sample and embodiment 5~8,10,11, A therein2B7Type phase containing magnesium and A5B19Type contains
The accounting of magnesium phase (two kinds) in the alloy is obviously improved.The heat treatment method provided through the invention has high hydrogen storage
The A of volumetric properties2B7Type Phase Proportion containing magnesium even more from far away be more than using prior heat treatment mode be heat-treated it is congruent
Alloy.Illustrate that the heat treatment method of hydrogen bearing alloy provided by the invention can overcome alloy Phase Proportion variation in heat treatment process to become
The shortcomings that gesture is unable to control realizes that effective, direction explicitly contains the control of magnesium Phase Proportion, improves alloying component, the stabilization of performance
Property.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (9)
1. a kind of heat treatment method of the volatile metal hydrogen storage alloy containing low melting point characterized by comprising it is easy low melting point will to be contained
Volatilized metal hydrogen bearing alloy and compensation are heat-treated simultaneously in closed container.
2. the heat treatment method of the volatile metal hydrogen storage alloy according to claim 1 containing low melting point, which is characterized in that institute
Stating compensation is the metal product containing the low-melting-point metal.
3. the heat treatment method of the volatile metal hydrogen storage alloy according to claim 2 containing low melting point, which is characterized in that institute
State compensation and the mass ratio containing the low-melting-point metal in the volatile metal hydrogen storage alloy of low melting point be 0.0005~
0.5:1。
4. the heat treatment method of the volatile metal hydrogen storage alloy according to claim 1 containing low melting point, which is characterized in that institute
Stating low-melting-point metal includes at least one of Mg, Sm, Nd, Al, Sm, Sn and Zn.
5. the heat treatment method of the volatile metal hydrogen storage alloy according to claim 1 containing low melting point, which is characterized in that institute
Stating heat treatment method includes: to carry out heat to the volatile metal hydrogen storage alloy containing low melting point under conditions of 800~1000 DEG C
Processing.
6. the heat treatment method of the volatile metal hydrogen storage alloy according to claim 5 containing low melting point, which is characterized in that right
The time that the volatile metal hydrogen storage alloy containing low melting point is heat-treated is 2~20h.
7. the heat treatment method of the volatile metal hydrogen storage alloy according to claim 1 containing low melting point, which is characterized in that institute
State the inside that closed container is set to heat-treatment furnace, the closed container includes cabinet and the case lid that matches with the cabinet,
The case lid is covered on the opening of the cabinet.
8. the heat treatment method of the volatile metal hydrogen storage alloy according to claim 7 containing low melting point, which is characterized in that institute
It states cabinet and the case lid junction is equipped with sealing element.
9. the heat treatment method of the volatile metal hydrogen storage alloy as claimed in any one of claims 1 to 8 containing low melting point is manufacturing
Application in solid hydrogen storage device and nickel-metal hydride battery.
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| CN201811092864.5A CN109136799B (en) | 2018-09-18 | 2018-09-18 | Heat treatment method and application of hydrogen storage alloy containing low-melting-point volatile metal |
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| CN201811092864.5A CN109136799B (en) | 2018-09-18 | 2018-09-18 | Heat treatment method and application of hydrogen storage alloy containing low-melting-point volatile metal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111270056A (en) * | 2020-03-06 | 2020-06-12 | 武汉理工大学 | Method for heat treatment of alloy containing volatile element in saturated steam environment of the element |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113497A (en) * | 2006-07-25 | 2008-01-30 | 北京有色金属研究总院 | Method for preparing RE-Mg-Ni-M series hydrogen storage alloy |
| 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 |
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2018
- 2018-09-18 CN CN201811092864.5A patent/CN109136799B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113497A (en) * | 2006-07-25 | 2008-01-30 | 北京有色金属研究总院 | Method for preparing RE-Mg-Ni-M series hydrogen storage alloy |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111270056A (en) * | 2020-03-06 | 2020-06-12 | 武汉理工大学 | Method for heat treatment of alloy containing volatile element in saturated steam environment of the element |
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Address after: 510000 363 Changxin Road, Tianhe District, Guangzhou, Guangdong. Patentee after: Institute of rare metals, Guangdong Academy of Sciences Address before: 510000 363 Changxin Road, Tianhe District, Guangzhou, Guangdong. Patentee before: GUANGDONG INSTITUTE OF RARE METALS |
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Effective date of registration: 20230324 Address after: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee after: Institute of resource utilization and rare earth development, Guangdong Academy of Sciences Address before: 510000 363 Changxin Road, Tianhe District, Guangzhou, Guangdong. Patentee before: Institute of rare metals, Guangdong Academy of Sciences |