CN103789573A - Zr-based Laves phase hydrogen storage alloy and preparation method thereof - Google Patents
Zr-based Laves phase hydrogen storage alloy and preparation method thereof Download PDFInfo
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- CN103789573A CN103789573A CN201410027987.6A CN201410027987A CN103789573A CN 103789573 A CN103789573 A CN 103789573A CN 201410027987 A CN201410027987 A CN 201410027987A CN 103789573 A CN103789573 A CN 103789573A
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Abstract
The invention discloses a Zr-based Laves phase hydrogen storage alloy and a preparation method thereof. The Zr-based Laves phase hydrogen storage alloy comprises 30 at. percent of Zr, 3.33 at. percent of Ti, totally 66.67 at. percent of V and Al including 1.33-16.67 at. percent of Al, and the balance of vanadium. The chemical formula of the Zr-based Laves phase hydrogen storage alloy is Zr0.9Ti0.1(V(1-x)Alx)2(x=0.02, 0.05, 0.10, 0.15 and 0.25) and is prepared through melting and vacuum annealing. On the basis of an AB2 ZrV2 alloy, a Ti element replaces A-side Zr element, and Al replaces a B-side V element; a uniform Laves phase is prepared from the alloy through the vacuum annealing; due to the Al element, the stability of an alloy hydride is lowered, the hysteresis effect of the hydrogen storage alloy in a hydrogen absorption and desorption process is improved, and the performance of the alloy is improved. The Zr-based Laves phase hydrogen storage alloy also has the characteristics of simple and feasible technology, high efficiency, low equipment requirement and low cost.
Description
Technical field
The present invention relates to alloy material storing hydrogen technical field, be specifically related to a kind of ultralow equilibrium pressure AB
2type Zr-Ti-V-Al hydrogen storage alloy and preparation method thereof.
Background technology
Hydrogen storage material is as a kind of novel functional materials and the energy, the feature such as it has, and hydrogen-storage amount is large, energy consumption is low, environment compatibility is good, operating pressure is low, easy to use.Find LaNi since middle 1960s
5since the reversible hydrogen storage effect of the intermetallic compounds such as FeTi, hydrogen storage alloy and applied research thereof are developed rapidly.Oneself is widely used in storage and the transportation of hydrogen, the separation that hydrogen coordination is tired, temperature and pressure sensor, the fields such as nickel-hydrogen chargeable cell in recent years.
Hydrogen isotope tritium and deuterium have a wide range of applications in nuclear energy field, but it is as radioactive hydrogen isotropic substance, in use must strictly control.Then, in actually operating, unavoidable generation containing tritium waste gas, can not directly discharge, and need go out tritium processing.Hydrogen storage alloy is for detritiation device, have simple in structure, economical convenient, safety coefficient is high, compares with at present main detritiation technique hydride process, does not produce the advantages such as secondary pollutant HTO, zirconium base Laves phase hydrogen storage alloy is large with its hydrogen-storage amount, the advantages such as hydrogen absorption equilibrium pressure is low, easily-activated, existing own certain applications are in this field.Although it is better compared with magnesium system and group of the lanthanides that zirconium base Laves phase hydrogen storage alloy is inhaled hydrogen dynamic performance, also need further improvement, and its hydride is too stable, be difficult for decomposing, while putting hydrogen, there is obvious lag-effect in suction.
In the preparation of Zr base Laves phase hydrogen storage alloy, alloying is to reduce the main path of its hydride Enthalpies of Formation.Alloying to a certain degree can be improved the suction hydrogen desorption kinetics performance of Zr base Laves phase hydrogen storage alloy, and can in suction hydrogen discharge reaction temperature, play crucial katalysis.By adjusting ratio and the M-H bonding strength inhaling hydrogen in alloy and do not inhale protium, improve suction and put hydrogen thermodynamics and kinetics performance, carry heavy alloyed sucking/placing hydrogen amount.By adjusting the crystalline structure of alloy, control alloy hydrogen absorption and desorption plateau pressure and hysteretic properties.By changing surface composition and the structure of alloy, improve alloy conductive performance and electrocatalysis characteristic, and improve the resistance to corrosion of alloy, improve alloy cycle life.
Metal A l is proved the suction hydrogen desorption kinetics performance that can effectively improve Zr base alloy, adds Al element simultaneously and can reduce the stability of alloy hydride.Adopt Al to substitute V, be expected to improve the suction hydrogen desorption kinetics of Zr base Laves phase hydrogen storage alloy and improve its suction and put the lag-effect in hydrogen process.
Summary of the invention
For overcoming the AB existing in prior art
2type Zr base Laves phase hydrogen storage alloy is inhaled the deficiency of hydrogen dynamic performance, and it is excessive that hydrogen hysteresis quality is put in suction, the present invention proposes a kind of Zr base Laves phase hydrogen storage alloy and preparation method thereof.
Zr-Ti-V-Al hydrogen storage alloy of the present invention is by core level sponge Zr piece, Ti plate and V crystal, by chemical formula Zr
0.9ti
0.1(V
0.75～0.98al
0.25～0.02)
2formulated; Described ratio is atomic ratio.
The purity of described core level sponge Zr piece is 99.4%, and the purity of described Ti plate is 99.97%, and the purity of described V crystal is 99.5%.
A kind of method that the invention allows for the Zr of preparation base Laves phase hydrogen storage alloy, material preparation method is specific as follows:
The present invention is at AB
2type ZrV
2on alloy basis, use respectively Ti element substitution A side Zr element, with the alternative B side V element of Al, advantage is specific as follows:
1, aspect prepared by hydrogen storage alloy, hydrogen storage alloy ingot is by non-consumable arc melting, carries out at water jacketed copper crucible, and because cooling rate is very fast, process of setting belongs to nonequilibrium freezing, and alloy reaction is incomplete, tends to exist Peritectic Reaction residual phase in cast alloy.And by further homogenizing annealing processing for a long time, making rich vanadium solid solution phase and α-Zr in alloy that solid solution reaction further occur mutually, alloy obtains more uniform Laves phase.
2, it is simple for process that the method is prepared Zr-base hydrogenous alloy, and efficiency is high, low for equipment requirements, and cost is low.
3, the interpolation of Al element has increased the diffusion admittance of hydrogen atom, has accelerated hydrogen molecule and has resolved into hydrogen atom at alloy surface, has therefore improved ZrV
2alloy hydrogen absorption and desorption dynamic performance.Al element can lower the stability of alloy hydride, improves hydrogen storage alloy and puts the lag-effect in hydrogen process in suction, and its performance is as Fig. 2 and Fig. 3.
4, alloy of the present invention is ultralow equilibrium pressure hydrogen storage alloy, and its equilibrium at room temperature pressure platform is lower than 10
-10pa, the advantage such as highest attainable vacuum ability is strong, to the operating mode such as separation and recovery of hydrogen and hydrogen isotope under ultralow equilibrium pressure condition, has very large application advantage.
Table 1Zr
0.9ti
0.1(V
1-xal
x)
2the thermodynamical coordinate of hydrogen storage alloy and room temperature extrapolation equilibrium pressure
Accompanying drawing explanation
Fig. 1 is the Zr-Ti-V-Al hydrogen storage alloy as cast condition sample after silica tube Vacuum Package;
Fig. 2 is Zr-Ti-V-Al hydrogen storage alloy annealed state sample SEM photo;
Wherein: (a) (b) (c) (d) (e) be respectively Zr
0.9ti
0.1(V
0.98al
0.02)
2, Zr
0.9ti
0.1(V
0.95al
0.05)
2, Zr
0.9ti
0.1(V
0.9al
0.1)
2, Zr
0.9ti
0.1(V
0.85al
0.15)
2, Zr
0.9ti
0.1(V
0.75al
0.25)
2sEM photo after alloy sample annealing;
Fig. 3 is Zr-Ti-V-Al hydrogen storage alloy as cast condition (a) and annealed state (b) X-ray diffractogram;
Fig. 4 is first hydrogen curve (a) and the 773K Dynamic isotherms of hydrogen absorption (b) inhaled after the activation of Zr-Ti-V-Al hydrogen storage alloy;
Fig. 5 is Zr-Ti-V-Al hydrogen storage alloy P-C-T curve of hydrogen absorption;
Wherein: (a) (b) (c) (d) (e) be respectively Zr
0.9ti
0.1(V
0.98al
0.02)
2, Zr
0.9ti
0.1(V
0.95al
0.05)
2, Zr
0.9ti
0.1(V
0.9al
0.1)
2, Zr
0.9ti
0.1(V
0.85al
0.15)
2, Zr
0.9ti
0.1(V
0.75al
0.25)
2the P-C-T curve of alloy;
Fig. 6 is Van ' the t Hoff regression straight line of Zr-Ti-V-Al alloy;
Wherein: (a) (b) (c) (d) (e) be respectively Zr
0.9ti
0.1(V
0.98al
0.02)
2, Zr
0.9ti
0.1(V
0.95al
0.05)
2, Zr
0.9ti
0.1(V
0.9al
0.1)
2, Zr
0.9ti
0.1(V
0.85al
0.15)
2, Zr
0.9ti
0.1(V
0.75al
0.25)
2van ' the t Hoff regression straight line of alloy;
Fig. 7 is schema of the present invention.
Embodiment
Embodiment 1:
The present embodiment is a kind of Zr-Ti-V-Al hydrogen storage alloy, and the core level sponge Zr piece that described Zr-Ti-V-Al hydrogen storage alloy is 99.4% by purity, 99.97% Ti plate and 99.5% V crystal, by chemical formula Zr
0.9ti
0.1(V
0.98al
0.02)
2formulated, described ratio is atomic ratio.
The present embodiment has also proposed a kind of method of preparing described Zr-Ti-V-Al hydrogen storage alloy, and detailed process is:
As shown in Figure 2, after homogenizing annealing is processed, in alloy structure, rich V sosoloid dentrite quantity obviously reduces.In conjunction with the X-ray diffractogram of alloy before and after annealing shown in Fig. 3, can draw, in the time of homogenizing annealing, Zr
0.9ti
0.1(V
0.98al
0.02)
2alloy generation solid solution changes, and the dephasign quantity in alloy is able to obvious minimizing.After homogenizing annealing, alloy structure becomes more even.
Zr-Ti-V-Al hydrogen storage alloy ingot after annealing is cut into the thin slice of Φ 0.8mm × 1mm by machining, with acetone clean surface greasy dirt, then sample surfaces polishing, dehydrated alcohol are cleaned, dry final vacuum encapsulation.
Tested Zr-Ti-V-Al hydrogen storage alloy thin slice after annealing hydrogen storage property, result is as shown in Figure 4 and Figure 5.Zr
0.9ti
0.1(V
0.98al
0.02)
2activation performance of hydrogen-storage alloy is better, through 723K vacuum activating after 1 hour in the time that 303K inhales hydrogen first when incubation period compole short, hydrogen－sucking amount reaches 2.25wt.%; When 773K inhales hydrogen, can in 30 seconds, reach and inhale hydrogen running balance, show as good dynamic performance; Suction hydrogen P-C-T test selection 673K, 723K, 773K and tetra-temperature of 823K of alloy, put hydrogen P-C-T test selection 823K(as Fig. 5), alloy Hydrogen desorption isotherms overlaps with inhaling hydrogen curve, without putting hydrogen hysteresis phenomenon; Can determine by the slope of thermodynamics fit line with in the intercept (as Fig. 6) of Y-axis the thermodynamical coordinate that absorption hydrogen reacts, by thermodynamical coordinate substitution Van ' t Hoff equation, can try to achieve the hydrogen absorption equilibrium pressure of alloy under arbitrary temp.In table 1, list Zr
0.9ti
0.1(V
0.98al
0.02)
2the room temperature hydrogen absorption equilibrium pressure value of alloy under different hydrogen－sucking amounts, extrapolation equilibrium at room temperature forces down in 10
-12pa.
The present embodiment is a kind of Zr-Ti-V-Al hydrogen storage alloy, and the core level sponge Zr piece that described Zr-Ti-V-Al hydrogen storage alloy is 99.4% by purity, 99.97% Ti plate and 99.5% V crystal, by chemical formula Zr
0.9ti
0.1(V
0.95al
0.05)
2formulated, described ratio is atomic ratio.
The present embodiment has also proposed a kind of method of preparing described Zr-Ti-V-Al hydrogen storage alloy, and detailed process is:
As shown in Figure 2, after homogenizing annealing is processed, in alloy structure, rich V sosoloid dentrite quantity obviously reduces.In conjunction with the X-ray diffractogram of alloy before and after annealing shown in Fig. 3, can draw, in the time of homogenizing annealing, Zr
0.9ti
0.1(V
0.95al
0.05)
2alloy generation solid solution changes, and the dephasign quantity in alloy is able to obvious minimizing.After homogenizing annealing, alloy structure becomes more even.
Zr-Ti-V-Al hydrogen storage alloy ingot after annealing is cut into the thin slice of Φ 0.8mm × 1mm by machining, with acetone clean surface greasy dirt, then sample surfaces polishing, dehydrated alcohol are cleaned, dry final vacuum encapsulation.
Tested Zr-Ti-V-Al hydrogen storage alloy thin slice after annealing hydrogen storage property, result is as shown in Figure 4 and Figure 5.Zr
0.9ti
0.1(V
0.95al
0.05)
2activation performance of hydrogen-storage alloy is better, through 723K vacuum activating after 1 hour in the time that 303K inhales hydrogen first when incubation period compole short, hydrogen－sucking amount reaches 2.19wt.%; When 773K inhales hydrogen, can in 30 seconds, reach and inhale hydrogen running balance, show as good dynamic performance; Suction hydrogen P-C-T test selection 673K, 723K, 773K and tetra-temperature of 823K of alloy, put hydrogen P-C-T test selection 823K(as Fig. 5), alloy Hydrogen desorption isotherms overlaps with inhaling hydrogen curve, without putting hydrogen hysteresis phenomenon; Can determine by the slope of thermodynamics fit line with in the intercept (as Fig. 6) of Y-axis the thermodynamical coordinate that absorption hydrogen reacts, by thermodynamical coordinate substitution Van ' t Hoff equation, can try to achieve the hydrogen absorption equilibrium pressure of alloy under arbitrary temp.In table 1, list Zr
0.9ti
0.1(V
0.95al
0.05)
2the room temperature hydrogen absorption equilibrium pressure value of alloy under different hydrogen－sucking amounts, extrapolation equilibrium at room temperature forces down in 10
-13pa.
The present embodiment is a kind of Zr-Ti-V-Al hydrogen storage alloy, and the core level sponge Zr piece that described Zr-Ti-V-Al hydrogen storage alloy is 99.4% by purity, 99.97% Ti plate and 99.5% V crystal, by chemical formula Zr
0.9ti
0.1(V
0.9al
0.1)
2formulated, described ratio is atomic ratio.
The present embodiment has also proposed a kind of method of preparing described Zr-Ti-V-Al hydrogen storage alloy, and detailed process is:
As shown in Figure 2, after homogenizing annealing is processed, in alloy structure, rich V sosoloid dentrite quantity obviously reduces.In conjunction with the X-ray diffractogram of alloy before and after annealing shown in Fig. 3, can draw, in the time of homogenizing annealing, Zr
0.9ti
0.1(V
0.9al
0.1)
2alloy generation solid solution changes, and the dephasign quantity in alloy is able to obvious minimizing.After homogenizing annealing, alloy structure becomes more even.
Zr-Ti-V-Al hydrogen storage alloy ingot after annealing is cut into the thin slice of Φ 0.8mm × 1mm by machining, with acetone clean surface greasy dirt, then sample surfaces polishing, dehydrated alcohol are cleaned, dry final vacuum encapsulation.
Tested Zr-Ti-V-Al hydrogen storage alloy thin slice after annealing hydrogen storage property, result is as shown in Figure 4 and Figure 5.Zr
0.9ti
0.1(V
0.9al
0.1)
2activation performance of hydrogen-storage alloy is better, through 723K vacuum activating after 1 hour in the time that 303K inhales hydrogen first when incubation period compole short, hydrogen－sucking amount reaches 2.10wt.%; When 773K inhales hydrogen, can in 30 seconds, reach and inhale hydrogen running balance, show as good dynamic performance; Suction hydrogen P-C-T test selection 673K, 723K, 773K and tetra-temperature of 823K of alloy, put hydrogen P-C-T test selection 823K(as Fig. 5), alloy Hydrogen desorption isotherms overlaps with inhaling hydrogen curve, without putting hydrogen hysteresis phenomenon; Can determine by the slope of thermodynamics fit line with in the intercept (as Fig. 6) of Y-axis the thermodynamical coordinate that absorption hydrogen reacts, by thermodynamical coordinate substitution Van ' t Hoff equation, can try to achieve the hydrogen absorption equilibrium pressure of alloy under arbitrary temp.In table 1, list Zr
0.9ti
0.1(V
0.9al
0.1)
2the room temperature hydrogen absorption equilibrium pressure value of alloy under different hydrogen－sucking amounts, extrapolation equilibrium at room temperature forces down in 10
-9pa.
The present embodiment is a kind of Zr-Ti-V-Al hydrogen storage alloy, and the core level sponge Zr piece that described Zr-Ti-V-Al hydrogen storage alloy is 99.4% by purity, 99.97% Ti plate and 99.5% V crystal, by chemical formula Zr
0.9ti
0.1(V
0.85al
0.15)
2formulated, described ratio is atomic ratio.
The present embodiment has also proposed a kind of method of preparing described Zr-Ti-V-Al hydrogen storage alloy, and detailed process is:
As shown in Figure 2, after homogenizing annealing is processed, in alloy structure, rich V sosoloid dentrite quantity obviously reduces.In conjunction with the X-ray diffractogram of alloy before and after annealing shown in Fig. 3, can draw, in the time of homogenizing annealing, Zr
0.9ti
0.1(V
0.85al
0.15)
2alloy generation solid solution changes, and the dephasign quantity in alloy is able to obvious minimizing.After homogenizing annealing, alloy structure becomes more even.
Zr-Ti-V-Al hydrogen storage alloy ingot after annealing is cut into the thin slice of Φ 0.8mm × 1mm by machining, with acetone clean surface greasy dirt, then sample surfaces polishing, dehydrated alcohol are cleaned, dry final vacuum encapsulation.
Tested Zr-Ti-V-Al hydrogen storage alloy thin slice after annealing hydrogen storage property, result is as shown in Figure 4 and Figure 5.Zr
0.9ti
0.1(V
0.85al
0.15)
2activation performance of hydrogen-storage alloy is better, through 723K vacuum activating after 1 hour in the time that 303K inhales hydrogen first when incubation period compole short, hydrogen－sucking amount reaches 2.01wt.%; When 773K inhales hydrogen, can in 30 seconds, reach and inhale hydrogen running balance, show as good dynamic performance; Suction hydrogen P-C-T test selection 673K, 723K, 773K and tetra-temperature of 823K of alloy, put hydrogen P-C-T test selection 823K(as Fig. 5), alloy Hydrogen desorption isotherms overlaps with inhaling hydrogen curve, without putting hydrogen hysteresis phenomenon; Can determine by the slope of thermodynamics fit line with in the intercept (as Fig. 6) of Y-axis the thermodynamical coordinate that absorption hydrogen reacts, by thermodynamical coordinate substitution Van ' t Hoff equation, can try to achieve the hydrogen absorption equilibrium pressure of alloy under arbitrary temp.In table 1, list Zr
0.9ti
0.1(V
0.85al
0.15)
2the room temperature hydrogen absorption equilibrium pressure value of alloy under different hydrogen－sucking amounts, extrapolation equilibrium at room temperature forces down in 10
-10pa.。
The present embodiment is a kind of Zr-Ti-V-Al hydrogen storage alloy, and the core level sponge Zr piece that described Zr-Ti-V-Al hydrogen storage alloy is 99.4% by purity, 99.97% Ti plate and 99.5% V crystal, by chemical formula Zr
0.9ti
0.1(V
0.25al
0.75)
2formulated, described ratio is atomic ratio.
The present embodiment has also proposed a kind of method of preparing described Zr-Ti-V-Al hydrogen storage alloy, and detailed process is:
As shown in Figure 2, after homogenizing annealing is processed, in alloy structure, rich V sosoloid dentrite quantity obviously reduces.In conjunction with the X-ray diffractogram of alloy before and after annealing shown in Fig. 3, can draw, in the time of homogenizing annealing, Zr
0.9ti
0.1(V
0.25al
0.75)
2alloy generation solid solution changes, and the dephasign quantity in alloy is able to obvious minimizing.After homogenizing annealing, alloy structure becomes more even.
Zr-Ti-V-Al hydrogen storage alloy ingot after annealing is cut into the thin slice of Φ 0.8mm × 1mm by machining, with acetone clean surface greasy dirt, then sample surfaces polishing, dehydrated alcohol are cleaned, dry final vacuum encapsulation.
Tested Zr-Ti-V-Al hydrogen storage alloy thin slice after annealing hydrogen storage property, result is as shown in Figure 4 and Figure 5.Zr
0.9ti
0.1(V
0.25al
0.75)
2activation performance of hydrogen-storage alloy is better, through 723K vacuum activating after 1 hour in the time that 303K inhales hydrogen first when incubation period compole short, hydrogen－sucking amount reaches 1.98wt.%; When 773K inhales hydrogen, can in 30 seconds, reach and inhale hydrogen running balance, show as good dynamic performance; Suction hydrogen P-C-T test selection 673K, 723K, 773K and tetra-temperature of 823K of alloy, put hydrogen P-C-T test selection 823K(as Fig. 5), alloy Hydrogen desorption isotherms overlaps with inhaling hydrogen curve, without putting hydrogen hysteresis phenomenon; Can determine by the slope of thermodynamics fit line with in the intercept (as Fig. 6) of Y-axis the thermodynamical coordinate that absorption hydrogen reacts, by thermodynamical coordinate substitution Van ' t Hoff equation, can try to achieve the hydrogen absorption equilibrium pressure of alloy under arbitrary temp.In table 1, list Zr
0.9ti
0.1(V
0.25al
0.75)
2the room temperature hydrogen absorption equilibrium pressure value of alloy under different hydrogen－sucking amounts, extrapolation equilibrium at room temperature forces down in 10
-10pa.
Claims (3)
1. a Zr base Laves phase hydrogen storage alloy, is characterized in that, described Zr-Ti-V-Al hydrogen storage alloy is by core level sponge Zr piece, Ti plate and V crystal, by chemical formula Zr
0.9ti
0.1(V
0.75～0.98al
0.25～0.02)
2formulated; Described ratio is atomic ratio.
2. a kind of Zr base Laves phase hydrogen storage alloy as claimed in claim 1, is characterized in that, the purity of described core level sponge Zr piece is 99.4%, and the purity of described Ti plate is 99.97%, and the purity of described V crystal is 99.5%.
3. a method of preparing Zr base Laves phase hydrogen storage alloy described in claim 1, is characterized in that, detailed process is:
Step 1, melting; Load weighted starting material are put into water jacketed copper crucible, according to a conventional method to load weighted starting material melting; In melting, be evacuated to 6 × 10
-3, argon atmosphere protection is lower carries out alloy melting at vacuum non-consumable arc-melting furnace; In melting, by the hydrogen storage alloy ingot upset remelting obtaining 4 times;
Step 2, Vacuum Package; As cast condition hydrogen storage alloy ingot is cleaned and removes surperficial greasy dirt; Pack sample into silica tube, at 150～200 ℃ by silica tube bakeout degassing; Vacuumize processing by diffusion pump, when vacuum tightness reaches 10
-4when Pa magnitude, silica tube is sealed;
Step 3, homogenizing annealing processing; The as cast condition hydrogen storage alloy ingot that vacuum seal is installed is put into chamber type electric resistance furnace, is heated to 1273K and is incubated 168 hours; Insulation finishes rear furnace cooling with homogenizing annealing, obtains hydrogen storage alloy ingot.
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Cited By (3)
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| CN110042304A (en) * | 2019-04-22 | 2019-07-23 | 宁夏大学 | A kind of high-pressure metal hydride composite hydrogen occluding tank high platform pressure hydrogen bearing alloy |
| CN111118378A (en) * | 2019-12-31 | 2020-05-08 | 西安西工大超晶科技发展有限责任公司 | High-entropy alloy for nuclear and preparation method thereof |
| CN112779439A (en) * | 2021-01-28 | 2021-05-11 | 桂林电子科技大学 | Hydrogen storage material doped with V and capable of improving performance of ZrCo hydrogen storage alloy and preparation method of hydrogen storage material |
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| CN108411182B (en) * | 2018-04-13 | 2020-05-05 | 江苏理工学院 | Zr-Ti-Cr-V complex phase hydrogen storage alloy and preparation method thereof |
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