CN118147488A - TiCu phase enhanced AB2Ti-based alloy material and preparation method and application thereof - Google Patents
TiCu phase enhanced AB2Ti-based alloy material and preparation method and application thereof Download PDFInfo
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- CN118147488A CN118147488A CN202410282647.1A CN202410282647A CN118147488A CN 118147488 A CN118147488 A CN 118147488A CN 202410282647 A CN202410282647 A CN 202410282647A CN 118147488 A CN118147488 A CN 118147488A
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- 239000000956 alloy Substances 0.000 title claims abstract description 65
- 229910010165 TiCu Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000001257 hydrogen Substances 0.000 claims abstract description 49
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 49
- 239000011232 storage material Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims description 23
- 230000008018 melting Effects 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 23
- 238000003860 storage Methods 0.000 abstract description 14
- 238000005272 metallurgy Methods 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000006356 dehydrogenation reaction Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 210000001503 joint Anatomy 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 47
- 239000010949 copper Substances 0.000 description 14
- 239000011651 chromium Substances 0.000 description 12
- 239000011572 manganese Substances 0.000 description 11
- 230000001681 protective effect Effects 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 229910001068 laves phase Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 229910052704 radon Inorganic materials 0.000 description 2
- SYUHGPGVQRZVTB-UHFFFAOYSA-N radon atom Chemical compound [Rn] SYUHGPGVQRZVTB-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010169 TiCr Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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Abstract
The invention provides a TiCu phase enhanced AB 2 type Ti-based alloy material, a preparation method and application thereof, and belongs to the technical field of hydrogen storage materials. The structural formula is as follows: ti 1.1‑xZrxCr1.2Mn0.8‑yCuy; wherein x is 0.05-0.15, and y is 0.1-0.3. According to the invention, after the A-side excess chemical quantity and Zr are adopted to replace Ti, the capacity of the alloy is effectively improved, and meanwhile, the platform pressure of the alloy is obviously reduced, and the thermodynamic performance of the alloy is improved. Under 283K, the hydrogen absorption capacity exceeds 1.6wt.%, the platform pressure is 7bar, and the solid hydrogen storage material is used as a solid hydrogen storage material of a medium-low pressure hydrogen pipeline, is used for butt joint of a hydrogen storage system and a hydrogenator/metallurgy, and has the advantages of large hydrogen storage capacity, small hysteresis, quick hydrogen absorption and release dynamics and low dehydrogenation platform pressure. The promotion of hydrogen metallurgy is beneficial to the purposes of energy conservation and environmental protection.
Description
Technical Field
The invention relates to the technical field of hydrogen storage materials, in particular to a TiCu phase reinforced AB 2 type Ti-based alloy material, a preparation method and application thereof.
Background
Hydrogen metallurgy is a clean revolutionary steel production technology that utilizes hydrogen instead of carbon as a metallurgical process fuel and reductant, and the reaction product is water. Compared with the traditional carbon metallurgy, the method can fundamentally reduce carbon emission and realize the clean production target.
The hydrogen supply end is upstream of the hydrogen metallurgy process, and the hydrogen storage system in the hydrogen supply end is the key of the whole hydrogen metallurgy process, and the performance of the hydrogen storage system is mainly determined by the hydrogen storage material. TiCr 2 is one of common hydrogen storage alloys, has a Laves phase structure, and has the advantages of fast dynamics and large hydrogen storage capacity. However, tiCr 2 has higher platform pressure and larger hysteresis, and is often required to be modified in an alloying mode and the like, so that the method is popularized and applied practically.
Disclosure of Invention
The invention aims to provide a TiCu phase reinforced AB 2 type Ti-based alloy material, and a preparation method and application thereof. The TiCu phase dispersed and separated in the smelting and cooling process improves the phase boundary density of the alloy and increases the hydrogen atom diffusion channel, so that the dynamics performance of the alloy is improved, and the obtained TiCu phase reinforced AB 2 type Ti-based alloy material has the advantages of large hydrogen storage capacity, small hysteresis, quick hydrogen absorption and desorption dynamics and low dehydrogenation platform pressure.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a TiCu phase reinforced AB 2 type Ti-based alloy material, which has the structural formula:
Ti1.1-xZrxCr1.2Mn0.8-yCuy；
wherein x is 0.05-0.15, and y is 0.1-0.3.
The invention also provides a preparation method of the TiCu phase reinforced AB 2 type Ti-based alloy material, which comprises the following steps:
And (3) mixing titanium, zirconium, chromium, manganese and copper in a protective atmosphere, and then carrying out arc melting to obtain the TiCu-phase reinforced AB 2 -type Ti-based alloy material.
Preferably, the temperature of the arc melting is more than or equal to 2000 ℃.
Preferably, the remelting times of the arc melting are more than or equal to 5 times, and the time of single arc melting is 50-70 s.
Preferably, the vacuum degree of the arc melting is less than or equal to 2.7X10 -3 Pa.
The invention also provides application of the TiCu phase enhanced AB 2 type Ti-based alloy material in a hydrogen storage material.
The invention has the following beneficial effects:
the invention provides a TiCu phase reinforced AB 2 type Ti-based alloy material, which has the structural formula:
Ti 1.1-xZrxCr1.2Mn0.8-yCuy; wherein x is 0.05-0.15, and y is 0.1-0.3. According to the invention, after the A-side excess chemical quantity and Zr are adopted to replace Ti, the capacity of the alloy is effectively improved, and meanwhile, the platform pressure of the alloy is obviously reduced, and the thermodynamic performance of the alloy is improved.
The TiCu-phase-reinforced AB 2 -based Ti-based alloy material provided by the invention has the advantages of high hydrogen storage capacity, small hysteresis, fast hydrogen absorption and desorption kinetics and low dehydrogenation platform pressure, and the hydrogen absorption capacity exceeds 1.6wt.% under 283K, the platform pressure is 7bar, and the TiCu-phase-reinforced AB 2 -based alloy material is used as a solid hydrogen storage material for a medium-low pressure hydrogen pipeline, is used for butt joint of a hydrogen storage system and a hydrogenator/metallurgy. The promotion of hydrogen metallurgy is beneficial to the purposes of energy conservation and environmental protection.
The invention also provides a preparation method of the TiCu phase reinforced AB 2 type Ti-based alloy material, which comprises the following steps: and (3) mixing titanium, zirconium, chromium, manganese and copper in a protective atmosphere, and then carrying out arc melting to obtain the TiCu-phase reinforced AB 2 -type Ti-based alloy material. The TiCu-phase reinforced AB 2 -based Ti-based alloy material can be prepared through vacuum arc melting, and the subsequent processes such as heat treatment and the like are not needed, so that the method is very simple and convenient.
Drawings
FIG. 1 is an XRD pattern of TiCu phase enhanced type AB 2 Ti-based alloy material of example 1;
FIG. 2 is a back-scattered image and an energy spectrum sweep image of TiCu phase enhanced AB 2 type Ti-based alloy material of example 1;
wherein (a) is a back-scattered image; (b) Energy spectrum surface scanning images of Ti, zr, cr, mn, cu respectively;
FIG. 3 is a pressure-composition-isotherm test plot of TiCu phase enhanced type AB 2 Ti-based alloy material of example 1;
FIG. 4 is a graph of the kinetics of TiCu phase enhanced type AB 2 Ti-based alloy material of example 1;
Fig. 5 is a graph of a hydrogen desorption van der joff fit of a TiCu phase enhanced AB 2 type Ti-based alloy material of example 1.
Detailed Description
The invention provides a TiCu phase reinforced AB 2 type Ti-based alloy material, which has the structural formula:
Ti 1.1-xZrxCr1.2Mn0.8-yCuy; wherein x is 0.05-0.15, and y is 0.1-0.3.
In the present invention, when x is between 0.05 and 0.1, hydrogen can be absorbed at 243K more than 1.8wt.%, and the plateau slope is less than 1.2.
In the present invention, when x is greater than 0.1, the plateau pressure is less than 8bar at 283K, and the hydrogen absorption amount exceeds 1.6wt.%.
In the present invention, y is preferably 0.12 to 0.28, more preferably 0.14 to 0.26, and still more preferably 0.16 to 0.24.
The invention also provides a preparation method of the TiCu phase reinforced AB 2 type Ti-based alloy material, which comprises the following steps:
And (3) mixing titanium, zirconium, chromium, manganese and copper in a protective atmosphere, and then carrying out arc melting to obtain the TiCu-phase reinforced AB 2 -type Ti-based alloy material.
In the invention, the protective atmosphere is formed by the following steps: and (5) after rough vacuumizing through a mechanical pump, cleaning by introducing protective gas. This step is cycled 4 times to form a protective atmosphere.
In the present invention, the shielding gas is preferably one or more of argon, helium, nitrogen, neon, xenon and radon, and the vacuum degree after rough evacuation by the mechanical pump is preferably 3 to 8Pa, more preferably 4 to 7Pa, and even more preferably 5Pa.
In the invention, after forming protective atmosphere, a molecular pump is started to vacuum until the vacuum degree is less than or equal to 2.7X10 -3 Pa, and then protective gas is introduced. The shielding gas is preferably one or more of argon, helium, nitrogen, neon, xenon and radon; the pressure of the reaction system after the shielding gas is introduced again is preferably 0.05 to 0.10MPa, more preferably 0.06 to 0.09MPa, and even more preferably 0.07 to 0.08MPa.
In the invention, the specific mode of arc melting is as follows: and (3) firstly striking an arc, and simultaneously heating and melting a pure zirconium block in the furnace chamber by using the arc to absorb residual oxygen in the furnace chamber, wherein each metal sample needs to be turned over for remelting.
In the present invention, the temperature of the arc melting is preferably not less than 2000 ℃, more preferably not less than 2200 ℃, and still more preferably not less than 2400 ℃.
In the present invention, the number of remelting times of the arc melting is preferably 5 or more, more preferably 6 or more, still more preferably 7 or more, and the time of single arc melting is preferably 50 to 70s, more preferably 55 to 65s, still more preferably 58 to 62s.
In the present invention, the vacuum degree of the arc melting is preferably not more than 2.7X10 -3 Pa, more preferably not more than 2.5X10 - 3 Pa, still more preferably not more than 2.4X10 -3 Pa.
In the invention, the TiCu phase reinforced AB 2 type Ti-based alloy material is obtained after cooling after arc melting. The cooling mode is preferably water cooling, and the time of the water cooling is preferably 15 to 25 minutes, more preferably 18 to 22 minutes, and even more preferably 19 to 21 minutes.
The invention also provides application of the TiCu phase enhanced AB 2 type Ti-based alloy material in a hydrogen storage material.
In the present invention, the preparation materials are commercially available as known to those skilled in the art unless otherwise specified.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) 3.5036G Ti, 0.6642g Zr, 4.5547g Cr, 3.0912gMn, 0.4671g Cu having a purity of 99.9% or more were placed in a copper crucible of a vacuum arc melting furnace. Closing a furnace cover, opening a mechanical pump to vacuum degree of 5Pa, filling argon to 0.05MPa, and opening the mechanical pump to vacuum to 5Pa. This step was repeated twice to form a protective atmosphere. The molecular pump is started to be vacuumized until the vacuum degree is 2.7 multiplied by 10 -3 Pa, argon is filled to the air pressure of 0.07MPa, and the mixture is smelted in an electric arc at 2500 ℃. Firstly, striking an arc, and simultaneously heating and melting pure zirconium blocks in a furnace chamber by using the arc to absorb residual oxygen in the furnace chamber. In order to improve the uniformity of the samples, each sample needs to be turned over and remelted for 5 times, the melting time is about 60s each time, and 11.9974g of alloy cast ingot is obtained after cooling by a water-cooled copper mold for 20 min.
(2) Polishing the alloy cast ingot obtained in the step (1) by using a grinder, so as to remove oxides on the surface of the alloy. The alloy was then crushed into powder in a glove box and sieved using a 200 mesh sieve to obtain the TiCu phase reinforced AB 2 type Ti-based alloy material Ti 1Zr0.1Cr1.2Mn0.7Cu0.1.
Crushing the alloy ingot in the step (1) in a glove box, sieving with a 400-mesh sieve, and performing XRD test on the obtained alloy powder; the test results are shown in FIG. 1, and it can be seen from FIG. 1 that the alloy exhibits a dual phase structure, which is a C14 Laves phase and a TiCu phase.
The block cast ingot is embedded with epoxy resin and then ground by a grinder, and ground on 300-mesh, 600-mesh, 1000-mesh, 1500-mesh and 2000-mesh gauze paper, and then is polished by a silicon dioxide polishing solution and subjected to analysis by a scanning electron microscope, and the result is shown in figure 2, wherein (a) is a back scattering image; (b) Energy spectrum facial scan images of Ti, zr, cr, mn, cu respectively: as can be seen from fig. 2, cu element in the alloy is biased, which is consistent with the XRD characterization result.
And (3) performing pressure-component-isotherm (PCI) test on the hydrogen storage material powder in the step (2), wherein the test instrument is a domestic 50 MPa-level hydrogen storage performance tester, the test temperature is 243-283K, the test pressure is 0.01-10 MPa, and the result is shown in figure 3, and the hydrogen release pressure of the alloy is 12bar under 283K.
The kinetics performance of the hydrogen storage material powder in the step (2) is tested under the conditions of 243K and 10MPa hydrogen pressure, and the result is shown in fig. 4, and as can be seen from fig. 4, the TiCu phase enhanced AB 2 type Ti-based alloy material Ti 1Zr0.1Cr1.2Mn0.7Cu0.1 absorbs 1.86wt.% hydrogen under the condition of 243K.
The PCI performance of the TiCu phase reinforced AB 2 type Ti-based alloy material prepared in example 1 was subjected to a van-terjov fit, and the result is shown in fig. 5: the enthalpy of hydrogen release of the alloy became 22.54kJ/mol.
Examples 2, 3 and comparative examples 1 to 3 were identical to example 1 in terms of the preparation method and reaction conditions, except for the mass ratios of titanium, zirconium, chromium, manganese and copper, as shown in Table 1.
TABLE 1 composition and thermodynamic Properties of alloy materials of examples 2 and 3 and comparative examples 1 to 3
As can be seen from Table 1, with the increase of the substitution amount of Zr to Ti, the hydrogen releasing platform pressure of the alloy at the same temperature is obviously reduced, and the hydrogen storage amount is improved. Therefore, proper Zr substitution in the TiCu phase reinforced AB 2 type Ti-based alloy material can improve the stability of hydride, reduce the hydrogen releasing platform pressure of the material, and is beneficial to the practical application of the TiCu phase reinforced AB 2 type Ti-based alloy material. As a preferred solution, the TiCu phase-reinforced AB 2 type Ti-based alloy material Ti 1Zr0.1Cr1.2Mn0.7Cu0.1 has the maximum hydrogen storage amount.
As can be seen from the above examples, the present invention provides a TiCu phase reinforced AB 2 type Ti-based alloy material, which has the structural formula: ti 1.1-xZrxCr1.2Mn0.8-yCuy; wherein x is 0.05-0.15, y is 0.1-0.3, and the embodiment of the invention effectively reduces the platform pressure of the alloy, improves the hydrogen storage capacity of the alloy, realizes the regulation and control of the hydrogen storage thermodynamic property of the alloy and obtains the high-performance TiCu phase enhanced AB 2 type Ti-based alloy material through the A side excess chemical quantity and the A/B side element substitution, especially the substitution of Ti by the A side Zr.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. The TiCu phase reinforced AB 2 type Ti-based alloy material is characterized by comprising the following structural formula:
Ti1.1-xZrxCr1.2Mn0.8-yCuy；
wherein x is 0.05-0.15, and y is 0.1-0.3.
2. The method for preparing the TiCu phase reinforced AB 2 type Ti-based alloy material according to claim 1, which is characterized by comprising the following steps:
Under the protection atmosphere, the TiCu phase reinforced AB 2 type Ti-based alloy material is obtained by arc melting after mixing metals according to the chemical composition in claim 1.
3. The method for preparing a TiCu phase reinforced AB 2 type Ti-based alloy material according to claim 2, wherein the arc melting temperature is equal to or higher than 2000 ℃.
4. The method for preparing a TiCu phase reinforced AB 2 type Ti-based alloy material according to claim 2 or 3, wherein the remelting times of arc melting is more than or equal to 5 times, and the single arc melting time is 50-70 s.
5. The method for producing a TiCu phase-reinforced AB 2 type Ti-based alloy material according to claim 4, wherein the vacuum degree of arc melting is 2.7X10 -3 Pa or less.
6. Use of the TiCu phase-reinforced AB 2 type Ti-based alloy material of claim 1 in hydrogen storage materials.
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| CN202410282647.1A CN118147488A (en) | 2024-03-12 | 2024-03-12 | TiCu phase enhanced AB2Ti-based alloy material and preparation method and application thereof |
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| CN202410282647.1A CN118147488A (en) | 2024-03-12 | 2024-03-12 | TiCu phase enhanced AB2Ti-based alloy material and preparation method and application thereof |
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