CN111575562A - Magnesium alloy cast body, method for producing same and use thereof - Google Patents
Magnesium alloy cast body, method for producing same and use thereof Download PDFInfo
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- CN111575562A CN111575562A CN202010282204.4A CN202010282204A CN111575562A CN 111575562 A CN111575562 A CN 111575562A CN 202010282204 A CN202010282204 A CN 202010282204A CN 111575562 A CN111575562 A CN 111575562A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to the technical field of materials, in particular to a magnesium alloy casting, a preparation method thereof and application thereof in hydrogen production by hydrolysis. The magnesium alloy casting comprises the following raw materials: cu element: 1-8 wt.%, Ni element: 3-14 wt.%, Gd element: 0-3 wt.%, Fe element: 0.5-2 wt.%, with the balance Mg, based on the total mass of the feedstock. The preparation method of the magnesium alloy comprises the following steps: (1) weighing various raw materials according to a predetermined weight percentage, and pretreating the raw materials for later use; (2) mixing the pretreated raw materials obtained in the step (1), and smelting under the protection of a covering agent to obtain a uniform melt; and then casting the uniform melt to obtain the magnesium alloy casting. The magnesium alloy casting disclosed by the invention has the advantages of excellent hydrogen production effect by hydrolysis, environmental friendliness, simple preparation method and suitability for popularization and application.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a magnesium alloy casting, a preparation method thereof and application thereof in hydrogen production by hydrolysis.
Background
Since the 20 th century and the 80 th century, with the rapid development of the world economy and the continuous increase of the global population, the world energy consumption also greatly rises, and main fossil fuels such as petroleum, natural gas and coal cannot meet the long-term requirement of the development of the world economy; and with the increasing deterioration of global environmental conditions and the increasing awareness of environmental protection of people in various countries, the traditional energy industry generating a large amount of harmful gases and wastes has been more and more difficult to meet the development requirements of human society.
Taking hydrogen energy as an example, it can be used as a potential clean energy source for fuel cells of automobiles, but at present, the application of hydrogen energy is not practically popularized, which may be related to the problems of low efficiency, small scale, poor environmental protection and the like existing in hydrogen energy preparation. Many researchers have conducted a great deal of research in terms of improvement of energy materials in order to develop more excellent hydrogen production materials, particularly materials capable of producing hydrogen through a simple hydrolysis reaction.
Metals and compounds are new hydrogen production materials by hydrolysis in recent years. At present, people have successively studied sodium (Na), aluminum (Al) and magnesium (Mg) element system materials, and the Mg metal hydrogen production has higher electrochemical activity, reduced solution pH value and simpler hydrogen production condition, and is more suitable for metal hydrolysis hydrogen production.
However, the magnesium (Mg) element system (MgH)2Mg or alloys thereof) still present hydrolysis by-products Mg (OH)2Easy to wrap MgH2The particles limit the hydrolysis reaction, for which the alloy structure is usually refined by a high-energy ball-milling process, the specific surface area is increased, the hydrogen-production kinetics are improved, or by the addition of active metal or compound elements, such as SnO2Rare earth RE, Mg2Ni、Mg2Si, graphene, noble metal elements Ga, In and the like, regulate and control the activity of the magnesium-based alloy, or eliminate Mg (OH) by using a catalytic substance or an acid salt solution or a salt solution In combination In hydrolysate2And the protective layer promotes the hydrogen production reaction. In other words, the magnesium-based hydrolysis hydrogen production material still has the following problems: the economic cost and the safe cost of the powder material preparation process are high; the reaction requires the elimination of Mg (OH) by the catalytic species2A protective layer; the existing bulk material has relatively high component and process cost and has certain environmental pollution (gallium)Indium).
Therefore, there is a need to develop a hydrogen production energy material and a preparation process thereof, which have the advantages of low cost, rapid reaction, high efficiency and environmental protection.
Disclosure of Invention
The present disclosure provides a magnesium alloy casting, which at least solves the problems of low hydrogen production efficiency and low hydrogen production speed of the existing hydrogen production materials.
The disclosure also provides a method for preparing the magnesium alloy casting, and the method has simpler process.
The disclosure also provides the application of the magnesium alloy casting in hydrolysis hydrogen production, and solves the problems of high safety cost and high material cost of the existing hydrogen production process.
One aspect of the present disclosure provides a magnesium alloy casting, which comprises the following raw materials:
cu element: 1-8 wt.%,
ni element: 3-14 wt.%,
gd element: 0-3 wt.%,
fe element: 0.5-2 wt.%,
the balance being Mg, based on the total mass of the raw materials.
In an embodiment of the magnesium alloy cast of the present disclosure, the Fe element may be present in the magnesium alloy cast in an ionic form or may be present in the magnesium alloy cast in an elemental form, provided that substantially all (0.5 to 2 wt.%) of the Fe element in the raw material is contained in the final magnesium alloy cast.
It is conceivable that the formulation of the magnesium alloy cast body of the present disclosure includes solid-dissolving as large an amount of Fe element as possible in the magnesium alloy containing Cu, Ni, Gd in order to promote the hydrolysis reaction of the magnesium alloy cast body to proceed more rapidly.
The magnesium alloy casting disclosed by the invention utilizes the interaction of Cu, Ni, Gd, Fe and Mg to promote the hydrolysis reaction, and the elements are low in price and environment-friendly.
In a further embodiment of the magnesium alloy cast of the present disclosure, the raw material of the magnesium alloy cast comprises the following components:
cu element: 1.4-3 wt.%,
ni element: 2-8 wt.%,
gd element: 1.2-3 wt.%,
fe element: 0.5-2 wt.%,
the balance being Mg, based on the total mass of the raw materials.
In still further embodiments of the magnesium alloy cast of the present disclosure, the raw material of the magnesium alloy cast comprises the following components:
cu element: 1.4-2.5 wt.%,
ni element: 2-4 wt.%,
gd element: 1.5-3 wt.%,
fe element: 0.5-1.5 wt.%,
the balance being Mg, based on the total mass of the raw materials.
In an embodiment of the magnesium alloy cast body of the present disclosure, the magnesium alloy cast body includes a second phase, the second phase is lamellar or flaky, and the crystal grain is large and the grain size reaches 70 to 100 μm. The lamellar or platelet shape of the second phase and its larger grains have impact, cutting hydrolysis products such as Mg (OH)2The formed protective layer has the function of further facilitating the contact of the unreacted part of the magnesium alloy and the hydrolysis medium after the protective layer is broken, so that the hydrolysis reaction speed is further improved.
In the magnesium alloy cast body of the present disclosure, the second phase may be a second phase formed of Cu, Ni, Gd, Fe element and Mg element, and may be, for example, Mg-Cu, Mg-Gd-Ni, Mg-Fe second phase.
In the magnesium alloy cast body of the present disclosure, the "cast body" is used to indicate that the magnesium alloy should be in a body shape, not in a powder shape (particle size 0.5 to 1 μm). In addition to the above limitations on the composition of the magnesium alloy of the present invention, the structure of the magnesium alloy is defined herein. In the case of "castings", hydrolysates such as Mg (OH)2The complete cladding is not easy to form on the surface of the magnesium alloy reactant, thereby further facilitating the contact of the magnesium alloy reactant and a hydrolysis medium and promoting the improvement of the hydrolysis reaction speed.
In an embodiment of the magnesium alloy cast body of the present disclosure, the magnesium alloy cast body is a magnesium alloy cast body produced by melting a raw material under the protection of a covering agent to obtain a homogeneous melt, followed by casting. In other words, the magnesium alloy of the present disclosure is a magnesium alloy obtained by direct casting of a homogeneous melt without further refining. It is contemplated that the design concept of the magnesium alloy casting of the present disclosure includes inclusion of impurities in the magnesium alloy, which are believed to facilitate the hydrolysis reaction of the magnesium alloy.
Yet another aspect of the present disclosure provides a method of producing the above magnesium alloy cast body, the method comprising the steps of:
(1) weighing various raw materials according to a predetermined weight percentage, and pretreating the raw materials for later use;
(2) mixing the pretreated raw materials obtained in the step (1), and smelting under the protection of a covering agent to obtain a uniform melt; and then casting the uniform melt to obtain the magnesium alloy casting.
In one embodiment of the disclosed manufacturing method, in step (1), the pretreatment comprises drying the raw material to remove moisture and humidity from the surface.
In one embodiment of the disclosed manufacturing method, in step (1), the raw material is selected from the group consisting of metallic magnesium, pure Cu, Mg-25Ni master alloy, Mg-30Gd master alloy, and FeCl3(ii) a Or selected from magnesium metal, Mg-30Cu, Mg-25Ni master alloy, Mg-30Gd master alloy and FeCl3。
In step (1), the Fe element is introduced in ionic form, for example as FeCl3The form is introduced, so that the solid solution amount of Fe element in the magnesium alloy can be improved, and Cl ions are introduced into the magnesium alloy. The magnesium alloy prepared by the method has very high hydrolysis speed even if reacting with pure water, which is probably related to the fact that the magnesium alloy disclosed by the invention can separate out Cl ions in the hydrolysis process.
In the preparation method of the present disclosure, in the step (2), the processes of feeding, heating and mixing of various raw materials can be performed by using a conventional operation method in the art. For example, a predetermined amount of magnesium metal can be melted by heating to 720-760 ℃ under the protection of the covering agent, and then addingInto pure Cu, Mg-25Ni master alloy, Mg-30Gd master alloy and FeCl3Stirring, heat preservation and melting. The higher smelting temperature is beneficial to the diffusion of elements such as Gd (gadolinium), Ni (nickel) and the like, and can better ensure that all elements are uniformly distributed in the molten liquid to reduce segregation.
The covering agent may be selected from conventional covering agents used in the art for this purpose. The stirring can be carried out in a manner conventional in the art for this purpose, for example by electromagnetic stirring. The stirring holding time may be, for example, 30 to 40min, provided that a homogeneous melt is obtained.
In the preparation method disclosed by the invention, in the step (2), a melt refining process can be omitted, and the magnesium alloy casting can be directly cast after being uniformly stirred, so that the process operation is saved, and meanwhile, the hydrolysis performance of the obtained magnesium alloy casting is more excellent.
In the preparation method of the present disclosure, in the step (2), the casting temperature is 700-740 ℃, for example 720-740 ℃. Higher casting temperatures may promote the formation of coarse grains, increasing the grain size of the second phase; and the blockage of the liquid conveying pipe due to the reduction of the fluidity of the solution after elements such as gadolinium and nickel are added can be avoided, and the smooth casting process is facilitated.
In the production method of the present disclosure, in step (2), the cooling rate may be appropriately slowed down after the casting. For example, the speed of pulling out the ingot by semi-continuous casting can be controlled to be 2-5mm/s, and the water amount can be controlled to be 800ml/s at 300-. Thus being beneficial to the growth of crystal grains, having low cooling speed and providing more sufficient time for the second phase to separate out and grow, thereby being beneficial to obtaining the magnesium alloy with better hydrolysis effect.
A further aspect of the present disclosure provides the use of a magnesium alloy casting as described above for the hydrolysis of hydrogen production.
As known to those skilled in the material art, magnesium alloys are mainly used as structural materials and exert certain mechanical properties, but are easily corroded to affect the use, so that research on magnesium alloys by those skilled in the material art is mainly focused on corrosion protection. In contrast, the inventors of the present disclosure conducted research in the opposite direction, and developed the magnesium alloy casting energy source material of the present disclosure for hydrolysis hydrogen production under the condition that the action relationship among different content and different kinds of alloy elements is unclear.
In an embodiment of the use of the present disclosure, the magnesium alloy casting is processed into a small volume and used in the form of a block or a plate when used for hydrogen production by hydrolysis. When the catalyst is used for hydrolysis reaction, the proper crushing into smaller volume is beneficial to increasing the specific surface area and promoting the hydrolysis application to be better played.
The scheme of the disclosure can achieve the following technical effects:
1. when the magnesium alloy casting body is used for hydrolysis hydrogen production reaction, a barrier film is not easily formed on the surface of the casting body, the reaction speed is high, the reaction solution can be pure water, chloride ion brine and seawater, the reaction can be carried out in a lower water temperature range such as 0-100 ℃, and a catalyst does not need to be added.
2. The raw materials of the alloying elements added in the magnesium alloy disclosed by the invention are low in price, and the preparation cost of the magnesium alloy is low.
3. The method for preparing the magnesium alloy for hydrolysis has simple process, easy actual operation and strong industrial popularization.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosure, and are incorporated in and constitute a part of this specification.
FIG. 1 is a sectional image of a magnesium alloy casting of the present disclosure.
Detailed Description
The present disclosure will be described in further detail with reference to the drawings and embodiments. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant disclosure and not restrictive of the disclosure.
Example 1
Selecting raw material block metal magnesium (the purity is more than or equal to 99.8 percent), pure Cu, Mg-25Ni intermediate alloy, Mg-30Gd intermediate alloy and FeCl3The components are weighed according to the following mass percentage: gadolinium (Gd): 2 wt%; copper (Cu): 1.5 wt%; nickel (Ni): 3 wt%; iron (Fe): 1 wt%; the balance being magnesium.
Then the raw materials are put into a drying furnace for drying, and the moisture and humidity on the surface are removed.
Under the protection of the covering agent, the temperature of the magnesium block is heated to 720-760 ℃ to melt the magnesium block. Then pure Cu, Mg-25Ni, Mg-30Gd intermediate alloy and FeCl3Putting the block into the magnesium solution, electromagnetically stirring and preserving heat for 30-40min to obtain uniform solution.
Then casting the molten liquid at the temperature of 700-720 ℃ under electromagnetic stirring to obtain the magnesium alloy casting body.
And then according to the needs, further preparing small blocks with the length multiplied by the width multiplied by the height multiplied by 1cm multiplied by 2cm multiplied by 3cm by means of mechanical grinding crushing or machining and the like, further increasing the surface area, and using the small blocks for preparing hydrogen by hydrolysis.
10g of the prepared magnesium alloy small block was put into pure water at 25 ℃ and the hydrogen yield, the hydrogen yield and the time to reach the maximum hydrogen yield were measured.
Patent CN205879719U is incorporated in its entirety into this disclosure as a measuring device for hydrogen production.
The measurement results are shown in table 1.
Example 2
A magnesium alloy casting is prepared according to the method in the embodiment 1, and the difference is that the addition amount of Fe element is increased, and the Fe element is weighed according to the following mass percentage: gadolinium (Gd): 2 wt%; copper (Cu): 1.5 wt%; nickel (Ni): 3 wt%; iron (Fe): 1.5 wt%; the balance being magnesium.
Hydrolysis hydrogen production measurements are shown in table 1.
Example 3
A magnesium alloy casting is prepared according to the method in the embodiment 1, and the difference is that the addition amount of Fe element is reduced, and the Fe element is weighed according to the following mass percentage: gadolinium (Gd): 2 wt%; copper (Cu): 1.5 wt%; nickel (Ni): 3 wt%; iron (Fe): 0.5 wt%; the balance being magnesium.
Hydrolysis hydrogen production measurements are shown in table 1.
Comparative example 1
The magnesium alloy casting prepared according to the embodiment 1 is different in that the selected raw materials do not contain Fe element, and specifically, the magnesium alloy casting is prepared by the following weight percentage: gadolinium: (Gd)2 wt%; copper (Cu): 1.5 wt%; nickel (Ni): 3 wt%; the balance being magnesium.
Hydrolysis hydrogen production measurements are shown in table 1.
Comparative example 2
The magnesium alloy casting is prepared according to the method in the embodiment 1, and the difference is that the selected raw materials do not contain Gd element, and specifically, the magnesium alloy casting is weighed according to the following mass percentage: copper (Cu): 1.5 wt%; nickel (Ni): 3 wt%; iron (Fe): 1 wt%; the balance being magnesium.
Hydrolysis hydrogen production measurements are shown in table 1.
Comparative example 3
A magnesium alloy casting was prepared as described in example 1, except that the Fe-containing material was selected to be pure iron, not FeCl3。
The results of the hydrogen production by hydrolysis are shown in Table 1
Comparative example 4
A magnesium alloy casting was produced as described in example 1, except that a refining step was added in the production process.
Concretely, pure Cu, Mg-25Ni, Mg-30Gd intermediate alloy and FeCl3Putting the block into the magnesium solution, electromagnetically stirring and preserving heat for 30-40min to obtain uniform solution, and then refining for 60-120 min. Then casting is carried out at the temperature of 700-720 ℃ under electromagnetic stirring to obtain the magnesium alloy casting.
Comparative example 5
A magnesium alloy cast was prepared as described in example 1, except that the magnesium alloy cast was ground into powder having a particle size of 0.5 to 1 μm, and subjected to hydrolysis hydrogen production reaction.
TABLE 1
It will be understood by those skilled in the art that the foregoing embodiments are merely for clarity of illustration of the disclosure and are not intended to limit the scope of the disclosure. Other variations or modifications may occur to those skilled in the art, based on the foregoing disclosure, and are still within the scope of the present disclosure.
Claims (10)
1. The magnesium alloy casting is characterized in that the raw materials comprise the following components:
cu element: 1-8 wt.%,
ni element: 3-14 wt.%,
gd element: 0-3 wt.%,
fe element: 0.5-2 wt.%,
the balance being Mg, based on the total mass of the raw materials.
2. The magnesium alloy cast according to claim 1, characterized in that the raw material comprises the following components:
cu element: 1.4-3 wt.%,
ni element: 2-8 wt.%,
gd element: 1.2-3 wt.%,
fe element: 0.5-2 wt.%,
the balance being Mg, based on the total mass of the raw materials.
3. The magnesium alloy cast according to claim 1, characterized in that the raw material comprises the following components:
cu element: 1.4-2.5 wt.%,
ni element: 2-4 wt.%,
gd element: 1.5-3 wt.%,
fe element: 0.5-1.5 wt.%,
the balance being Mg, based on the total mass of the raw materials.
4. The magnesium alloy cast according to any one of claims 1 to 3, characterized in that the magnesium alloy cast contains a second phase, and the second phase is lamellar or flaky.
5. The magnesium alloy cast according to any one of claims 1 to 3, characterized in that it is a magnesium alloy cast produced by melting raw materials under the protection of a covering agent to obtain a homogeneous melt followed by casting.
6. A method of producing a magnesium alloy cast according to any one of claims 1 to 5, characterized by comprising the steps of:
(1) weighing various raw materials according to a predetermined weight percentage, and pretreating the raw materials for later use;
(2) mixing the pretreated raw materials obtained in the step (1), and smelting under the protection of a covering agent to obtain a uniform melt; and then casting the uniform melt to obtain the magnesium alloy casting.
7. The method according to claim 6, wherein in step (1), the raw material is selected from the group consisting of metallic magnesium, pure Cu, Mg-25Ni master alloy, Mg-30Gd master alloy and FeCl3(ii) a Or selected from magnesium metal, Mg-30Cu, Mg-25Ni master alloy, Mg-30Gd master alloy and FeCl3。
8. The method according to claim 6 or 7, characterized in that in step (2), the casting is performed immediately after obtaining a homogeneous melt.
9. Use of magnesium alloy castings according to claims 1-5 for hydrolytic hydrogen production.
10. Use according to claim 9, characterized in that the magnesium alloy casting is processed to a small volume for use in block or plate form when used for hydrogen production by hydrolysis.
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Cited By (1)
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CN115198154A (en) * | 2022-07-12 | 2022-10-18 | 山东海化集团有限公司 | Magnesium alloy easy to store and transport and controllable in hydrogen production rate and preparation method and application thereof |
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CN115198154A (en) * | 2022-07-12 | 2022-10-18 | 山东海化集团有限公司 | Magnesium alloy easy to store and transport and controllable in hydrogen production rate and preparation method and application thereof |
CN115198154B (en) * | 2022-07-12 | 2023-10-20 | 山东海化集团有限公司 | Magnesium alloy easy to store and transport and controllable in hydrogen production rate, and preparation method and application thereof |
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