CN112111673A - Method for preparing aluminum alloy with fine grain characteristics and aluminum alloy prepared by same - Google Patents
Method for preparing aluminum alloy with fine grain characteristics and aluminum alloy prepared by same Download PDFInfo
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- CN112111673A CN112111673A CN201910532998.2A CN201910532998A CN112111673A CN 112111673 A CN112111673 A CN 112111673A CN 201910532998 A CN201910532998 A CN 201910532998A CN 112111673 A CN112111673 A CN 112111673A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/08—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents with metals
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a method for preparing aluminum alloy with fine grain characteristics and the prepared aluminum alloy, wherein the method comprises the steps of adding a rare earth refiner into a melt of a hydrolysable hydrogen-producing aluminum alloy under stirring in the process of smelting to prepare the hydrolysable hydrogen-producing aluminum alloy, uniformly mixing, cooling and forming to obtain a modified hydrolysable hydrogen-producing aluminum alloy; wherein the rare earth refiner is aluminum-cerium alloy, the addition amount of the rare earth refiner is 0.001-1 wt% of the weight of the modified hydrolyzable hydrogen-producing aluminum alloy, and the aluminum-cerium alloy comprises 76-92 wt% of aluminum and 8-24 wt% of cerium. The invention can effectively refine aluminum crystal grains in the aluminum alloy, thereby greatly improving the hydrolysis rate of the aluminum alloy.
Description
Technical Field
The invention belongs to the field of hydrolysis hydrogen production of aluminum alloy, and particularly relates to a method for preparing aluminum alloy with fine grain characteristics and the prepared aluminum alloy.
Background
The exhaustion of fossil energy and the environmental problems caused by combustion are receiving wide attention, and hydrogen energy is regarded as the most promising clean energy in the 21 st century, and particularly, the utilization rate of hydrogen energy can be improved by combining with the use of a fuel cell. The storage of hydrogen is an important technical bottleneck that limits the widespread use of fuel cells. In addition, safety issues and high costs in the transportation of hydrogen gas also limit the large-scale use of hydrogen energy.
In order to meet the application requirements of proton exchange membrane fuel cells, the corresponding field hydrogen production technology requires that the raw materials have higher hydrogen production capacity and higher hydrogen production rate instantly. Meanwhile, the method has the characteristics of mild reaction conditions, quick and convenient reaction, easy carrying and storage of raw materials and the like.
The hydrogen production of the aluminum-gallium alloy has the characteristics of mild reaction conditions, quick and convenient reaction, small volume, convenient storage and the like, and hydrogen can be quickly produced by utilizing the hydrogen production of the aluminum-gallium alloy:
2Al+6H2O＝2Al(OH)3+3H2↑
1gAl can yield 1.244L H according to the above chemical reaction equation2(standard conditions) the aluminum in the alloy is generally fully reacted. However, in the existing research on hydrogen production of aluminum-gallium alloy, the shape of aluminum crystal grains can significantly affect the hydrogen production performance of aluminum alloy, so the size of the aluminum crystal grains must be controlled in large-scale production.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing an aluminum alloy with fine grain characteristics and the aluminum alloy prepared thereby, so as to improve the hydrogen production performance of aluminum alloy capable of producing hydrogen through hydrolysis.
In order to achieve one aspect of the above object, the present invention provides a method for preparing an aluminum alloy with fine grain characteristics, which adopts the following technical scheme:
a method for preparing aluminum alloy with fine grain characteristics comprises the steps of adding a rare earth refiner into a melt of a hydrolysable hydrogen-producing aluminum alloy under stirring in the process of smelting to prepare the hydrolysable hydrogen-producing aluminum alloy, uniformly mixing, cooling and forming to obtain a modified hydrolysable hydrogen-producing aluminum alloy with refined aluminum grains; wherein the rare earth refiner is aluminum-cerium alloy, the addition amount of the rare earth refiner is 0.001-1 wt% of the weight of the modified hydrolyzable hydrogen-producing aluminum alloy, and the aluminum-cerium alloy comprises 76-92 wt% of aluminum and 8-24 wt% of cerium.
In the present invention, the aluminum alloy capable of producing hydrogen by hydrolysis may be those known in the art which can produce hydrogen by hydrolysis of aluminum in the alloy with water. According to the method of the present invention, preferably, the hydrolyzable hydrogen-producing aluminum alloy is an Al-Ga-In-Sn alloy; in one embodiment, the Al-Ga-In-Sn alloy consists of: 70-98 wt% Al, 0.5-10 wt% Ga, 0.3-12 wt% In, and 0.3-12 wt% Sn; in one embodiment, the Al-Ga-In-Sn alloy composition may be In the following more general ranges: 80-94 wt%, such as 82 wt%, 85 wt%, 88 wt%, 90 wt% or 92 wt% aluminum, 1 wt% -8 wt%, such as 2 wt%, 2.5 wt%, 3 wt%, 4 wt% or 5 wt% gallium, 1-8 wt%, such as 2 wt%, 3 wt%, 4 wt%, 5 wt% or 6 wt% In, and 1-8 wt%, such as 2 wt%, 3 wt%, 4 wt%, 5 wt% or 6 wt% Sn; in the above aluminum alloys, Ga, In and Sn do not participate In the hydrolysis reaction by themselves, but serve to promote the hydrolysis of aluminum, and thus those skilled In the art understand that hydrolysis is equally feasible when the aluminum content In the aluminum alloy is lower, but is not preferred due to poor economy. In one embodiment, the Al-Ga-In-Sn alloy contains 5-10 wt%, such as 6 wt% or 8 wt% or 9 wt% of In and Sn, wherein the ratio of In to Sn is 3: 1.
In the invention, the rare earth refiner is an aluminum-cerium alloy with lower cerium content, and the research shows that the rare earth refiner has a good refining/modifying effect on aluminum grains in the aluminum alloy; preferably, the cerium content in the aluminum-cerium alloy is 10-20 wt%, such as 12 wt%, 13 wt%, 15 wt%, 17 wt% or 18 wt%; the aluminum cerium alloy is added in an amount of 0.01 to 0.5 wt.%, preferably 0.05 to 0.5 wt.%, such as 0.02, 0.04, 0.08, 0.1, 0.2, 0.3, or 0.4, based on the weight of the modified hydrolyzable hydrogen producing aluminum alloy.
In the present invention, the aluminum cerium alloy may be added in the form of small blocks or larger particles, for example, in one embodiment, the particle size of the added aluminum cerium alloy is 40 mesh or larger, such as 20 mesh, 16 mesh, 10 mesh, 7 mesh or 4 mesh.
In one embodiment of the invention, the method comprises:
(1) putting corresponding raw materials into a smelting furnace according to a ratio in a protective atmosphere for smelting;
(2) and adding the aluminum-cerium alloy into a smelting furnace, stirring and smelting for 1-20min, and pouring into a mold for cooling and molding.
In the step (1), the raw material can be a metal raw material for preparing the Al-Ga-In-Sn alloy, or an existing Al-Ga-In-Sn alloy product which is subjected to smelting so as to introduce a rare earth refiner into the alloy In the subsequent step.
In step (1), the protective atmosphere is well known in the art, such as a nitrogen atmosphere or other inert atmosphere; the smelting time and temperature are suitable for the alloy to be fully smelted, and can be determined by those skilled in the art according to actual conditions, in one embodiment, the smelting time in the step (1) is 0.5-2h, such as 1h or 1.5h, and the smelting temperature is 700-1000 ℃, such as 800 ℃ or 900 ℃.
In the step (2), the aluminum cerium alloy is added and then stirred, and the stirring is controlled to ensure uniform mixing, and the control can be carried out by a person skilled in the art according to the actual situation; the smelting time is controlled to be 1-20min so as to better guarantee the modification/refinement effect of aluminum crystal grains in the formed alloy, further improve the hydrogen production performance of the alloy and prevent the effect of the refiner from weakening or losing efficacy; preferably, in step (2), the smelting time is 5-15min, such as 8, 10min or 12 min.
It will be understood by those skilled in the art that the impurity content of each raw material or alloy used is generally as small as possible, and in the present invention, the impurity content of each raw material or alloy used is preferably 1% or less, such as 0.1%.
The invention also provides the aluminum alloy prepared by the method.
Compared with the prior art, the invention has the following advantages:
according to the invention, a proper amount of rare earth refiner is introduced into the aluminum alloy capable of producing hydrogen through hydrolysis in a melting mode, so that the appearance of aluminum grains in the aluminum alloy can be changed, the aluminum grains are refined, for example, from about 45 micrometers to 21 micrometers, and the hydrolysis reaction of the aluminum alloy is further promoted; the aluminum alloy prepared by the method can directly react after contacting with water, the completion time of hydrolysis reaction is shortened on the premise of not reducing the total hydrogen production, the average hydrogen production rate is high, on-line hydrogen supply and real-time hydrogen supply can be met, the method is suitable for providing a high-purity hydrogen source for a proton exchange membrane fuel cell, the process is simple, and the method is suitable for large-scale production and application.
Drawings
FIG. 1 is a scanning electron micrograph of a rare earth refiner-added alloy sample of example 1; in the microstructure and structure of the characterized aluminum alloy ingot, aluminum crystal grains are columnar, and the average width is about 35.2 mu m.
FIG. 2 is a scanning electron micrograph of a rare earth refiner added alloy sample of example 2; wherein, in the microstructure and the structure of the characterized aluminum alloy ingot, aluminum crystal grains are columnar, and the average width is about 21.0 μm.
FIG. 3 is a scanning electron micrograph of an alloy sample of comparative example 1 to which no rare earth refiner was added; in the microstructure and structure of the characterized aluminum alloy ingot, aluminum crystal grains are columnar, and the average width is about 45.4 mu m.
FIG. 4 is a graph showing the instantaneous hydrogen production rates of the aluminum alloys of examples 1 to 2 and comparative example 1, and the time for completion of the hydrolysis reaction after modification is significantly shortened.
FIG. 5 is a scanning electron micrograph of a rare earth refiner added alloy sample of example 3; in the microstructure and structure of the characterized aluminum alloy ingot, aluminum crystal grains are columnar, and the average width is about 26.7 mu m.
FIG. 6 is a scanning electron micrograph of an alloy sample of comparative example 2 to which no rare earth refiner was added; in the microstructure and structure of the characterized aluminum alloy ingot, aluminum crystal grains are columnar, and the average width is about 44.4 mu m.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
Unless otherwise specified, the impurity content of the raw materials used below is not more than 0.1 wt%.
Example 1
The preparation method comprises the steps of taking 90 wt% of Al blocks with the purity of more than 99.9%, 2.5 wt% of Ga with the purity of more than 99.9%, 7.5 wt% of In and Sn with the purity of more than 99.9% (the atomic ratio of In to Sn is 3:1) as raw materials, smelting for 1h at 800 ℃ In a stirring furnace filled with nitrogen protection gas, adding 0.05 wt% of aluminum cerium alloy particles (the size of the aluminum cerium alloy particles is about 20-30 meshes, the composition is 80 wt.% of Al-20 wt.% of Ce) accounting for the total amount (namely the sum of the metal raw materials and the mass of the added aluminum cerium alloy is the same as below), stirring for 10 minutes, pouring the aluminum cerium alloy particles into a steel mold, and cooling and molding to obtain the refined alloy material.
And sampling and carrying out SEM measurement, wherein a scanning electron microscope image of the SEM measurement is shown in figure 1, and the microstructure and the structure of the aluminum alloy ingot are characterized in that aluminum crystal grains are columnar and have the average width of about 35.2 microns.
The hydrolysis reaction was carried out on 1g of the prepared aluminum alloy and distilled water at 50 ℃, and the measured hydrogen production performance by hydrolysis was shown in table 1.
Example 2
The refined alloy material is prepared by taking 90 wt% of Al blocks with the purity of more than 99.9%, 2.5 wt% of Ga with the purity of more than 99.9%, 7.5 wt% of In and Sn with the purity of more than 99.9% (the atomic ratio of In to Sn is 3:1) as raw materials, smelting for 1h at 800 ℃ In a stirring furnace filled with nitrogen protection gas, adding 0.15 wt% of aluminum-cerium alloy particles (the size is about 6-8 meshes, the composition is 80 wt% of Al-20 wt% of Ce) accounting for the total amount, stirring for 10min, pouring In a steel mould, cooling and molding.
And sampling and carrying out SEM measurement, wherein a scanning electron microscope image of the SEM measurement is shown in figure 2, and the microstructure and the structure of the aluminum alloy ingot are characterized in that aluminum crystal grains are columnar and have the average width of about 21.0 mu m.
The hydrolysis reaction was carried out on 1g of the prepared aluminum alloy and distilled water at 50 ℃, and the measured hydrogen production performance by hydrolysis was shown in table 1.
Comparative example 1
The alloy material is prepared by melting 90 wt% of Al blocks with the purity of more than 99.9%, 2.5 wt% of Ga with the purity of more than 99.9%, 7.5 wt% of In and Sn with the purity of more than 99.9% and the atomic ratio of In to Sn of 3:1 In a stirring furnace filled with nitrogen protection gas at 800 ℃ for 1h, continuously stirring for 10min, pouring into a steel mold, cooling and molding.
And sampling and carrying out SEM measurement, wherein a scanning electron microscope image of the SEM measurement is shown in figure 3, and the microstructure and the structure of the aluminum alloy ingot are characterized in that aluminum crystal grains are columnar and have the average width of about 45.4 microns.
The hydrolysis reaction was carried out on 1g of the prepared aluminum alloy and distilled water at 50 ℃, and the measured hydrogen production performance by hydrolysis was shown in table 1.
Example 3
85 wt% of Al block, 5 wt% of Ga, 10 wt% of In and Sn, wherein the atomic ratio of In to Sn is 3:1, smelting at 900 ℃ for 1h In a stirring furnace filled with nitrogen protection gas, adding 0.4 wt% of aluminum-cerium alloy particles (the size is about 6-8 meshes, the composition is 90 wt% of Al-10 wt% of Ce) In the total amount, continuously stirring for 12 minutes, pouring into a steel mould, and cooling and molding to obtain the refined alloy material.
And sampling and carrying out SEM measurement, wherein a scanning electron microscope image of the SEM measurement is shown in figure 5, and the microstructure and the structure of the aluminum alloy ingot are characterized in that aluminum crystal grains are columnar and have the average width of about 26.7 microns.
The hydrolysis reaction was carried out on 1g of the prepared aluminum alloy and distilled water at 50 ℃, and the measured hydrogen production performance by hydrolysis was shown in table 1.
Comparative example 2
The same as in example 3, except that no rare earth refiner was added.
And sampling and carrying out SEM measurement, wherein a scanning electron microscope image of the SEM measurement is shown in figure 6, and the microstructure and the structure of the aluminum alloy ingot are characterized in that aluminum crystal grains are columnar and have an average width of about 44.4 microns.
The hydrolysis reaction was carried out on 1g of the prepared aluminum alloy and distilled water at 50 ℃, and the measured hydrogen production performance by hydrolysis was shown in table 1.
TABLE 1 hydrogen-making performance of aluminum alloy by hydrolysis hydrogen production
Claims (8)
1. The method for preparing the aluminum alloy with fine grain characteristics is characterized by comprising the steps of adding a rare earth refiner into a melt of a hydrolysable hydrogen-producing aluminum alloy under stirring in the process of smelting to prepare the hydrolysable hydrogen-producing aluminum alloy, uniformly mixing, cooling and forming to obtain a modified hydrolysable hydrogen-producing aluminum alloy; wherein the rare earth refiner is aluminum-cerium alloy, the addition amount of the rare earth refiner is 0.001-1 wt% of the weight of the modified hydrolyzable hydrogen-producing aluminum alloy, and the aluminum-cerium alloy comprises 76-92 wt% of aluminum and 8-24 wt% of cerium.
2. The method of claim 1, wherein the hydrolysable hydrogen-producing aluminum alloy is an Al-Ga-In-Sn alloy.
3. The method of claim 1, wherein the Al-Ga-In-Sn alloy consists of: 70-98 wt% Al, 0.5-10 wt% Ga, 0.3-12 wt% In, and 0.3-12 wt% Sn; preferably, the Al-Ga-In-Sn alloy consists of: 80-94 wt% Al, 1-8 wt% Ga, 1-8 wt% In, and 1-8 wt% Sn.
4. The method of claim 2, wherein the aluminum cerium alloy has a cerium content of 10-20 wt%; the addition amount of the aluminum-cerium alloy accounts for 0.01-0.5 wt% of the weight of the modified hydrolysable hydrogen-producing aluminum alloy.
5. The method according to any one of claims 1-4, characterized in that the method comprises:
(1) putting corresponding raw materials into a smelting furnace according to a ratio in a protective atmosphere for smelting;
(2) and adding the aluminum-cerium alloy into a smelting furnace, stirring and smelting for 1-20min, and pouring into a mold for cooling and molding.
6. The method as claimed in claim 5, wherein the alloy melting time in step (1) is 0.5-2h, and the melting temperature is 700-1000 ℃.
7. The method according to claim 5 or 6, wherein in the step (2), the stirring time is 5-15 min.
8. An aluminium alloy, characterized in that it is produced according to the method of any one of claims 1-7.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8418435B2 (en) * | 2008-06-13 | 2013-04-16 | Nagi Hatoum | Method for production of power from aluminum |
| CN104561673A (en) * | 2014-12-30 | 2015-04-29 | 长安大学 | Rare-earth-modified aluminium alloy anode plate and preparation method thereof |
| CN109295347A (en) * | 2018-05-31 | 2019-02-01 | 吉林大学 | One kind can be used for online hydrogen supply aluminum alloy materials |
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- 2019-06-19 CN CN201910532998.2A patent/CN112111673A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8418435B2 (en) * | 2008-06-13 | 2013-04-16 | Nagi Hatoum | Method for production of power from aluminum |
| CN104561673A (en) * | 2014-12-30 | 2015-04-29 | 长安大学 | Rare-earth-modified aluminium alloy anode plate and preparation method thereof |
| CN109295347A (en) * | 2018-05-31 | 2019-02-01 | 吉林大学 | One kind can be used for online hydrogen supply aluminum alloy materials |
Non-Patent Citations (2)
| Title |
|---|
| W. WANG等: "Investigation on microstructure and hydrogen generation performance of Al-rich alloys", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》 * |
| 马伯江等: "铝铈合金细化高纯铝", 《青岛科技大学学报(自然科学版)》 * |
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