CN113667908B - Nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material and preparation method thereof - Google Patents
Nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material and preparation method thereof Download PDFInfo
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- CN113667908B CN113667908B CN202111003741.1A CN202111003741A CN113667908B CN 113667908 B CN113667908 B CN 113667908B CN 202111003741 A CN202111003741 A CN 202111003741A CN 113667908 B CN113667908 B CN 113667908B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/005—Amorphous alloys with Mg as the major constituent
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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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
- C22C1/11—Making amorphous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C2200/00—Crystalline structure
- C22C2200/02—Amorphous
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/04—Hydrogen absorbing
Abstract
The invention relates to a nano TiF3And TiO2A nano-tube synergistically modified magnesium-based amorphous alloy hydrogen storage material and a preparation method thereof belong to the technical field of hydrogen storage materials. The nano TiF of the invention3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material: nano TiF with Mg-base amorphous alloy as base material3And TiO2The nanotube plays a role in coordination and modification, wherein the magnesium-based amorphous alloy is Mg-Ni-Rare Earth (RE) amorphous alloy. The invention adopts the quick quenching and low-energy ball milling modes to prepare the nano TiF3And TiO2The magnesium-based amorphous alloy hydrogen storage material cooperatively modified by the nanotube can ensure high hydrogen storage capacity of the amorphous alloy, promote high-efficiency dissociation and rapid diffusion of hydrogen molecules on the surface of the alloy into the alloy, and improve hydrogen absorption and desorption kinetics.
Description
Technical Field
The invention relates to a nano TiF3And TiO2A nano-tube synergistically modified magnesium-based amorphous alloy hydrogen storage material and a preparation method thereof belong to the technical field of hydrogen storage materials.
Background
Hydrogen energy is a new clean energy using hydrogen as a carrier, but the storage of hydrogen energy becomes a technical bottleneck for realizing hydrogen economy. Magnesium, low cost, abundant resources and considerable hydrogen storage capacity. However, the direct use of pure magnesium as a hydrogen storage medium not only has a high dehydrogenation temperature, but also has slow kinetics of hydrogen absorption and desorption. Ni and rare earth element RE are added by an alloying method to form a ternary alloy, and the ternary alloy is hydrogenated to form MgH2-Mg2NiH4-REHxThe nano-composite can greatly improve the effect.But at the same time, the hydrogen storage capacity ratio of pure magnesium is also greatly reduced.
The amorphous alloy is directly used as a hydrogen storage material, and has larger hydrogen storage capacity than the crystalline alloy; however, in order to ensure that the amorphous structure is not crystallized, the hydrogen absorption temperature needs to be below the crystallization temperature, which not only makes it difficult for hydrogen molecules to dissociate on the amorphous surface into hydrogen atoms to be absorbed by the hydrogen atoms, but also makes the hydrogen atoms lack diffusion channels and have slow hydrogen absorption and desorption kinetics.
Disclosure of Invention
Aiming at the problems of amorphous hydrogen storage materials in the prior art, the invention provides a nano TiF3And TiO2The nanotube synergistically modified Mg-based amorphous alloy hydrogen storage material is prepared by adopting a rapid quenching and low-energy ball milling mode to prepare nano TiF3And TiO2The magnesium-based amorphous alloy hydrogen storage material cooperatively modified by the nanotube can ensure high hydrogen storage capacity of the amorphous alloy, promote high-efficiency dissociation and rapid diffusion of hydrogen molecules on the surface of the alloy into the alloy, and improve hydrogen absorption and desorption kinetics.
Nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material: nano TiF with Mg-base amorphous alloy as base material3And TiO2The nano tube is a modifier, wherein the magnesium-based amorphous alloy is Mg-Ni-rare earth RE amorphous alloy;
by taking the mass of the magnesium-based amorphous alloy as 100%, 60-98% of magnesium, 1-20% of nickel and 1-20% of rare earth element RE; the rare earth element is one or more of yttrium, lanthanum, neodymium, praseodymium and holmium;
the nano TiF3And TiO2The total mass of the nano tube accounts for 2-10% of that of the magnesium-based amorphous alloy, and the nano TiF3Occupy nanometer TiF3And TiO210-90% of the total mass of the nanotube;
the nano TiF3And TiO2The preparation method of the nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material comprises the following specific steps:
(1) adding a magnesium ingot, a nickel ingot and a rare earth ingot into a smelting furnace for smelting, and cooling to obtain an alloy ingot;
(2) removing an oxide film on the surface of the alloy cast ingot, then melting the alloy cast ingot into an alloy melt, blowing the alloy melt onto the surface of a rotating roller by high-pressure inert gas for quick quenching treatment, and throwing out an amorphous magnesium-based alloy thin strip or an amorphous magnesium-based alloy filament;
(3) cutting amorphous magnesium-based alloy thin strip or amorphous magnesium-based alloy filament into amorphous magnesium-based alloy fragments, adding modifier nano TiF3And TiO2Nano tube, ball milling modified amorphous magnesium base alloy to obtain nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material;
the rotating speed of the roller in the step (2) is 20-50 m/s;
the ball-material ratio of ball milling in the step (3) is 10-50: 1, the rotating speed is 150-250 rpm, and the time is 1-5 h.
The invention has the beneficial effects that:
(1) the invention nanometer TiF3And TiO2The magnesium-based amorphous alloy hydrogen storage material cooperatively modified by the nanotube has large hydrogen storage capacity: the amorphous alloy obtained by rapid quenching is directly used as a hydrogen storage medium and has larger hydrogen storage capacity compared with the crystalline alloy;
(2) the invention nanometer TiF3And TiO2Nano TiF in nano tube synergistic modified magnesium base amorphous alloy hydrogen storage material3With TiO2The nanotube synergy has considerable hydrogen absorption and desorption kinetics: nano TiF3Hydrogen molecules can be efficiently dissociated to form a large number of active hydrogen atoms; TiO 22The special tubular structure of the nanotube provides a diffusion channel for hydrogen atoms obtained by dissociation, and the hydrogen atoms can easily pass through and diffuse into the amorphous alloy; nano TiF3With TiO2Compounds of Ti with the valence of +3 and +4 respectively, the catalyst of the multi-valence Ti can be used as a medium for electron transfer and promotes the electron transfer during the hydrogen absorption and desorption reaction; thus, nano TiF3And TiO2The hydrogen absorption and desorption rate is greatly improved by the synergistic catalytic action of the nano tube, and the hydrogen absorption and desorption dynamics are improved;
(3) the invention nanometer TiF3And TiO2Nanotube co-modificationThe magnesium-based amorphous alloy hydrogen storage material has good oxidation resistance: the disordered structure of the amorphous alloy has excellent oxidation resistance, while the conventional crystalline magnesium alloy is easy to oxidize at normal temperature, and a layer of oxide film generated on the surface not only causes the loss of hydrogen storage capacity, but also greatly reduces the hydrogen storage kinetic performance.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: nano TiF3And TiO2The preparation method of the nanotube synergistically modified magnesium-nickel-yttrium amorphous alloy hydrogen storage material comprises the following specific steps:
(1) adding a magnesium ingot, a nickel ingot and an yttrium ingot into an induction smelting furnace, smelting for 5min, and cooling to obtain an alloy ingot; based on the mass of the magnesium-based amorphous alloy as 100%, 98% of magnesium, 1% of nickel and 1% of rare earth element yttrium;
(2) polishing to remove oxide films on the surfaces of the alloy ingots, then placing the alloy ingots in a medium-frequency induction coil of an induction smelting furnace, heating and melting the alloy melts into alloy melts, blowing the alloy melts to the surfaces of rotating rollers through high-pressure argon gas for quick quenching treatment, and throwing out amorphous magnesium-based alloy filaments; wherein the rotating speed of the rollers is 40 m/s;
(3) cutting amorphous magnesium-based alloy filaments into amorphous magnesium-based alloy fragments, placing the amorphous magnesium-based alloy fragments in a ball milling tank, and adding a modifier of nano TiF3And TiO2Nano tube, ball milling modified amorphous magnesium base alloy, sieving with 200 mesh sieve to obtain nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material; wherein the amorphous magnesium-based alloy chips are 90 wt.%, and the nano TiF3In an amount of 5 wt.%, TiO2The adding amount of the nano tube is 5 wt.%, the ball-material ratio of ball milling is 20:1, the rotating speed is 200rpm, and the time is 3 h;
nano TiF3Hydrogen molecules can be efficiently dissociated to form a large number of active hydrogen atoms; TiO 22The special tubular structure of the nanotube provides a diffusion channel for hydrogen atoms obtained by dissociation, and the hydrogen atoms can easily pass through and diffuse into the amorphous alloy; nano TiF3With TiO2Compounds of Ti with the valence of +3 and +4 respectively, the catalyst of the multi-valence Ti can be used as a medium for electron transfer and promotes the electron transfer during the hydrogen absorption and desorption reaction; nano TiF3And TiO2The hydrogen absorption and desorption rate is greatly improved by the synergistic catalytic action of the nano tube, and the hydrogen absorption and desorption dynamics are improved.
Example 2: nano TiF3And TiO2The preparation method of the nanotube synergistically modified magnesium-nickel-lanthanum amorphous alloy hydrogen storage material comprises the following specific steps:
(1) adding a magnesium ingot, a nickel ingot and a lanthanum ingot into an induction smelting furnace, smelting for 7min, and cooling to obtain an alloy ingot; based on the mass of the magnesium-based amorphous alloy as 100%, 90% of magnesium, 5% of nickel and 5% of rare earth element lanthanum;
(2) polishing to remove an oxide film on the surface of the alloy ingot, then placing the alloy ingot in a medium-frequency induction coil of an induction smelting furnace to be heated and melted into an alloy melt, blowing the alloy melt onto the surface of a rotating roller by high-pressure argon gas to carry out quick quenching treatment, and throwing out an amorphous magnesium-based alloy thin strip; wherein the rotating speed of the rollers is 30 m/s;
(3) cutting the amorphous magnesium-based alloy thin strip into amorphous magnesium-based alloy fragments, placing the amorphous magnesium-based alloy fragments into a ball milling tank, and adding a modifier of nano TiF3And TiO2Nano tube, ball milling modified amorphous magnesium base alloy, sieving with 200 mesh sieve to obtain nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material; wherein the amorphous magnesium-based alloy chips are 92 wt.%, and the nano TiF3Is added in an amount of 3 wt.%, TiO2The adding amount of the nano tube is 5 wt.%, the ball-material ratio of the ball mill is 30:1, the rotating speed is 150rpm, and the time is 4 h;
nano TiF3Hydrogen molecules can be efficiently dissociated to form a large number of active hydrogen atoms; TiO 22The special tubular structure of the nanotube provides a diffusion channel for hydrogen atoms obtained by dissociation, and the hydrogen atoms can easily pass through and diffuse into the amorphous alloy; nano TiF3With TiO2Compounds of Ti with the valence of +3 and +4 respectively, the catalyst of the multi-valence Ti can be used as a medium for electron transfer and promotes the electron transfer during the hydrogen absorption and desorption reaction; nano TiF3And TiO2Of nanotubesThe hydrogen absorption and desorption speed is greatly improved under the synergistic catalysis effect, and the hydrogen absorption and desorption dynamics are improved.
Example 3: nano TiF3And TiO2The preparation method of the nanotube synergistically modified magnesium-nickel-neodymium amorphous alloy hydrogen storage material comprises the following specific steps:
(1) adding a magnesium ingot, a nickel ingot and a neodymium ingot into an induction smelting furnace, smelting for 8min, and cooling to obtain an alloy ingot; based on the mass of the magnesium-based amorphous alloy as 100%, 80% of magnesium, 10% of nickel and 10% of rare earth element neodymium;
(2) polishing to remove an oxide film on the surface of the alloy ingot, then placing the alloy ingot in a medium-frequency induction coil of an induction smelting furnace to be heated and melted into an alloy melt, blowing the alloy melt onto the surface of a rotating roller by high-pressure argon gas to carry out quick quenching treatment, and throwing out an amorphous magnesium-based alloy thin strip; wherein the rotating speed of the rollers is 40 m/s;
(3) cutting the amorphous magnesium-based alloy thin strip into amorphous magnesium-based alloy fragments, placing the amorphous magnesium-based alloy fragments into a ball milling tank, and adding a modifier of nano TiF3And TiO2Nano tube, ball milling modified amorphous magnesium base alloy, sieving with 200 mesh sieve to obtain nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material; wherein the amorphous magnesium-based alloy chips are 95 wt.%, and the nano TiF3In an amount of 2 wt.%, TiO2The adding amount of the nano tube is 3 wt.%, the ball-material ratio of the ball mill is 28:1, the rotating speed is 180rpm, and the time is 3.5 h;
nano TiF3Hydrogen molecules can be efficiently dissociated to form a large number of active hydrogen atoms; TiO 22The special tubular structure of the nanotube provides a diffusion channel for hydrogen atoms obtained by dissociation, and the hydrogen atoms can easily pass through and diffuse into the amorphous alloy; nano TiF3With TiO2Compounds of Ti with the valence of +3 and +4 respectively, the catalyst of the multi-valence Ti can be used as a medium for electron transfer and promotes the electron transfer during the hydrogen absorption and desorption reaction; nano TiF3And TiO2The hydrogen absorption and desorption rate is greatly improved by the synergistic catalytic action of the nano tube, and the hydrogen absorption and desorption dynamics are improved.
Example 4: nano TiF3And TiO2Nanotube synergistically modified Mg-Ni-Pr-Ho nonThe preparation method of the crystalline alloy hydrogen storage material comprises the following specific steps:
(1) adding a magnesium ingot, a nickel ingot, a praseodymium ingot and a holmium ingot into an induction smelting furnace, smelting for 10min, and cooling to obtain an alloy ingot; by taking the mass of the magnesium-based amorphous alloy as 100%, 60% of magnesium, 20% of nickel, 10% of rare earth element praseodymium and 10% of rare earth element holmium;
(2) polishing to remove an oxide film on the surface of the alloy ingot, then placing the alloy ingot in a medium-frequency induction coil of an induction smelting furnace to be heated and melted into an alloy melt, blowing the alloy melt onto the surface of a rotating roller by high-pressure argon gas to carry out quick quenching treatment, and throwing out an amorphous magnesium-based alloy thin strip; wherein the rotating speed of the rollers is 35 m/s;
(3) cutting the amorphous magnesium-based alloy thin strip into amorphous magnesium-based alloy fragments, placing the amorphous magnesium-based alloy fragments into a ball milling tank, and adding a modifier of nano TiF3And TiO2Nano tube, ball milling modified amorphous magnesium base alloy, sieving with 200 mesh sieve to obtain nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material; wherein the amorphous magnesium-based alloy chips are 96 wt.%, and the nano TiF3In an amount of 2 wt.%, TiO2The adding amount of the nano tube is 2 wt.%, the ball-material ratio of the ball mill is 25:1, the rotating speed is 250rpm, and the time is 3 h;
nano TiF3Hydrogen molecules can be efficiently dissociated to form a large number of active hydrogen atoms; TiO 22The special tubular structure of the nanotube provides a diffusion channel for hydrogen atoms obtained by dissociation, and the hydrogen atoms can easily pass through and diffuse into the amorphous alloy; nano TiF3With TiO2Compounds of Ti with the valence of +3 and +4 respectively, the catalyst of the multi-valence Ti can be used as a medium for electron transfer and promotes the electron transfer during the hydrogen absorption and desorption reaction; nano TiF3And TiO2The hydrogen absorption and desorption rate is greatly improved by the synergistic catalytic action of the nano tube, and the hydrogen absorption and desorption dynamics are improved.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (3)
1. Nano TiF3And TiO2The magnesium-based amorphous alloy hydrogen storage material cooperatively modified by the nanotube is characterized in that: nano TiF with Mg-base amorphous alloy as base material3And TiO2The nano tube is a modifier, wherein the magnesium-based amorphous alloy is Mg-Ni-rare earth RE amorphous alloy; by taking the mass of the magnesium-based amorphous alloy as 100%, 60-98% of magnesium, 1-20% of nickel and 1-20% of rare earth element RE; the rare earth element is one or more of yttrium, lanthanum, neodymium, praseodymium and holmium; nano TiF3And TiO2The total mass of the nano tube accounts for 2-10% of that of the magnesium-based amorphous alloy, and the nano TiF3Occupy nanometer TiF3And TiO210-90% of the total mass of the nanotube;
the preparation method of the magnesium-based amorphous alloy hydrogen storage material comprises the following specific steps:
(1) adding a magnesium ingot, a nickel ingot and a rare earth ingot into a smelting furnace for smelting, and cooling to obtain an alloy ingot;
(2) removing an oxide film on the surface of the alloy cast ingot, then melting the alloy cast ingot into an alloy melt, blowing the alloy melt onto the surface of a rotating roller by high-pressure inert gas for quick quenching treatment, and throwing out an amorphous magnesium-based alloy thin strip or an amorphous magnesium-based alloy filament;
(3) cutting amorphous magnesium-based alloy thin strip or amorphous magnesium-based alloy filament into amorphous magnesium-based alloy fragments, adding modifier nano TiF3And TiO2Nano tube, ball milling modified amorphous magnesium base alloy to obtain nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material; wherein the ball-material ratio of ball milling is 10-50: 1, the rotating speed is 150-250 rpm, and the time is 1-5 h.
2. The nano-TiF of claim 13And TiO2The preparation method of the nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material is characterized by comprising the following specific steps of:
(1) adding a magnesium ingot, a nickel ingot and a rare earth ingot into a smelting furnace for smelting, and cooling to obtain an alloy ingot;
(2) removing an oxide film on the surface of the alloy cast ingot, then melting the alloy cast ingot into an alloy melt, blowing the alloy melt onto the surface of a rotating roller by high-pressure inert gas for quick quenching treatment, and throwing out an amorphous magnesium-based alloy thin strip or an amorphous magnesium-based alloy filament;
(3) cutting amorphous magnesium-based alloy thin strip or amorphous magnesium-based alloy filament into amorphous magnesium-based alloy fragments, adding modifier nano TiF3And TiO2Nano tube, ball milling modified amorphous magnesium base alloy to obtain nano TiF3And TiO2Nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material.
3. The nano-TiF of claim 23And TiO2The preparation method of the nanotube synergistically modified magnesium-based amorphous alloy hydrogen storage material is characterized by comprising the following steps: and (3) the rotating speed of the roller in the step (2) is 20-50 m/s.
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