CN115807180A - Hydrogen storage alloy containing yttrium and its preparation process - Google Patents
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Abstract
The invention discloses a hydrogen storage alloy containing yttrium and a preparation process thereof. The yttrium-containing hydrogen storage alloy has the following composition: la m M n Y p Ca q Ni α Mn β Q γ (I) (ii) a Wherein M is selected from one or more of Ce, pr, nd, sm and Eu; q is selected from one or more of Cu, sn, V, ti, zr, cr, zn, mo and Si; it is composed ofIn the formula, m is more than or equal to 0.1 and less than or equal to 0.6, n is more than or equal to 0 and less than or equal to 0.5, p is more than or equal to 0.05 and less than or equal to 0.5, q is more than or equal to 0.1 and less than or equal to 0.4, and m + n + p + q =1; alpha is more than or equal to 4.6 and less than or equal to 4.95, beta is more than or equal to 0.05 and less than or equal to 0.4, gamma is more than or equal to 0 and less than or equal to 0.2, and alpha, beta and gamma are more than or equal to 4.95 and less than or equal to 5.2; wherein m, n, p, q, alpha, beta and gamma represent the mole fraction of each element respectively. The capacity retention rate of the yttrium-containing hydrogen storage alloy after being recycled is high.
Description
Technical Field
The invention relates to a hydrogen storage alloy containing yttrium and a preparation process thereof.
Background
The rare earth hydrogen storage alloy is an important energy conversion material for developing a hydrogen energy storage technology, and is mainly used as a negative electrode active material of a nickel-metal hydride battery and a hydrogen absorption/desorption medium of a solid hydrogen storage device. The solid hydrogen storage device adopts metal hydride hydrogen storage materials as hydrogen storage media, has low pressure and high safety, can directly store hydrogen prepared by electrolyzing water, and does not need high-pressure compression.
CN101260547A discloses an AB 5 A hydrogen storage alloy. The hydrogen storage alloy A comprises La, ce, pr and Nd, and the B comprises Ni, co, al and Mn. In the formulation of the raw materials for forming the hydrogen occluding alloy, la 2 O 3 18.1wt% of CeO 2 8.54wt%, pr 2 O 3 0.73wt%, nd 2 O 3 2.46wt%, mnO 2 6.42wt% of Al 2 O 3 1.77wt%, co 2 O 3 11.17wt%, and the balance NiO. The AB 5 The A side elements of the hydrogen storage alloy are all rare earth elements.
CN101994030A discloses a rare earth system AB 5 A hydrogen occluding alloy of the type represented by the following general formula Ml (Ni) 1-x-y- w Co x Mn y Al z M w ) m N n Ml is La and at least one element selected from Ce, pr, nd, sm, gd, dy, mg, ti and Zr, M is at least one element selected from Cu, fe, si, ge, sn, cr, zn, B, V, W, mo, ta and Nb, and N is Ca and/or Y. The hydrogen storage alloy must contain Co.
Disclosure of Invention
In view of the above, an object of the present invention is to provide an yttrium-containing hydrogen storage alloy having a high capacity retention rate after recycling. Further, the hydrogen absorption capacity of the yttrium-containing hydrogen storage alloy is high. Further, the yttrium-containing hydrogen storage alloy has a low enthalpy of hydride formation and a hysteresis coefficient. Another object of the present invention is to provide a process for preparing the above-mentioned hydrogen storage alloy containing yttrium.
The technical purpose is realized by the following technical scheme.
In one aspect, the invention provides an yttrium-containing hydrogen storage alloy having a composition as shown below:
La m M n Y p Ca q Ni α Mn β Q γ (I)
wherein M is selected from one or more of Ce, pr, nd, sm and Eu; q is selected from one or more of Cu, sn, V, ti, zr, cr, zn, mo and Si;
wherein m is more than or equal to 0.1 and less than or equal to 0.6, n is more than or equal to 0 and less than or equal to 0.5, p is more than or equal to 0.05 and less than or equal to 0.5, q is more than or equal to 0.1 and less than or equal to 0.4, and m + n + p + q =1; alpha is more than or equal to 4.6 and less than or equal to 4.95, beta is more than or equal to 0.05 and less than or equal to 0.4, gamma is more than or equal to 0 and less than or equal to 0.2, and alpha, beta and gamma are more than or equal to 4.95 and less than or equal to 5.2;
wherein m, n, p, q, alpha, beta and gamma represent the mole fraction of each element respectively.
In accordance with the yttrium-containing hydrogen storage alloys of the present invention, preferably, M comprises one or more of Ce or Sm.
The yttrium-containing hydrogen storage alloy according to the present invention, preferably, M is selected from one of the elemental compositions shown below:
(1)Ce；
(2)Sm；
(3) Ce and Sm;
(4) Ce and Nd.
The yttrium-containing hydrogen storage alloy according to the present invention preferably has 0.1. Ltoreq. N.ltoreq.0.4.
The yttrium-containing hydrogen storage alloy according to the present invention preferably has 0.2. Ltoreq. M.ltoreq.0.5.
The yttrium-containing hydrogen storage alloy according to the present invention is preferably 0.1. Ltoreq. P.ltoreq.0.4.
The yttrium-containing hydrogen storage alloy according to the present invention is preferably 0.15. Ltoreq. Q.ltoreq.0.3.
The yttrium-containing hydrogen storage alloy according to the invention is preferably 4.7 ≦ α ≦ 4.95,0.08 ≦ β ≦ 0.3, a + b =5.
The yttrium-containing hydrogen storage alloy according to the present invention preferably has a composition of one of the following:
La 0.4 Y 0.4 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Sm 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 V 0.1 ；
La 0.4 Ce 0.3 Y 0.1 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.3 Y 0.1 Ca 0.2 Ni 4.8 Mn 0.1 Ti 0.1 ；
La 0.3 Ce 0.2 Sm 0.1 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.2 Ce 0.2 Nd 0.2 Y 0.2 Ca 0.2 Ni 4.85 Mn 0.15 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 V 0.1 ；
La 0.4 Ce 0.1 Y 0.2 Ca 0.3 Ni 4.9 Mn 0.1 ；
La 0.3 Ce 0.25 Y 0.2 Ca 0.25 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.1 Y 0.3 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.2 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 Cu 0.1 ；
La 0.5 Ce 0.1 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.2 Ce 0.2 Y 0.3 Ca 0.3 Ni 4.7 Mn 0.3 。
on the other hand, the invention provides a preparation process of the yttrium-containing hydrogen storage alloy, which comprises the following steps:
smelting a metal raw material in an inert atmosphere at the temperature of 1100-1600 ℃ and under the pressure of 0.01-0.1 MPa to form a master alloy; and (3) annealing the master alloy in an inert atmosphere under the conditions that the pressure is 0.01-0.1 MPa and the temperature is 800-1200 ℃ to obtain the yttrium-containing hydrogen storage alloy.
According to the invention, ca is replaced by La and Y with proper amount, ni is replaced by Mn with proper amount, and the hydrogen absorption side element and the non-hydrogen absorption side element are controlled at proper molar ratio, so that the capacity retention rate of the hydrogen storage alloy after recycling can be improved, and the hydrogen storage alloy has higher hydrogen absorption amount. The hydrogen absorption amount of the hydrogen storage alloy can be further improved by replacing part of Y with rare earth elements such as Ce, sm, nd and the like.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
< Hydrogen occluding alloy containing yttrium >
The yttrium-containing hydrogen storage alloy of the present invention has the following composition:
La m M n Y p Ca q Ni α Mn β Q γ (I)。
the yttrium-containing hydrogen storage alloy does not contain Mg. Preferably, the yttrium-containing hydrogen storage alloys of the present invention do not contain Fe and Co. According to one embodiment of the present invention, the yttrium-containing hydrogen storage alloy of the present invention contains no other components except for unavoidable impurities.
La represents a lanthanum element. m represents the molar fraction of La. M is more than or equal to 0.1 and less than or equal to 0.6; preferably, 0.2. Ltoreq. M.ltoreq.0.5; more preferably, 0.3. Ltoreq. M.ltoreq.0.4.
M is one or more of Ce, pr, nd, sm and Eu. Preferably, M comprises one or more of Ce or Sm. More preferably, M is selected from one of the elemental compositions shown below: (1) Ce; (2) Sm; (3) Ce and Sm; (4) Ce and Nd. The M element can further improve the hydrogen absorption amount of the yttrium-containing hydrogen storage alloy on the basis of keeping higher capacity retention rate after cyclic use.
n represents the mole fraction of the M element. N is more than or equal to 0 and less than or equal to 0.5. In certain embodiments n =0. In other embodiments, 0.1. Ltoreq. N.ltoreq.0.4; preferably, 0.2. Ltoreq. N.ltoreq.0.3. The dosage of the M element can further improve the hydrogen absorption quantity of the yttrium-containing hydrogen storage alloy on the basis of keeping higher capacity retention rate after cyclic use.
In certain embodiments, M is Ce and Sm. The molar ratio of Ce to Sm may be (1-3) to 1; preferably (1.5-2.5) 1; more preferably 2. In other embodiments, M is Ce and Nd. The molar ratio of Ce to Nd may be (0.5-2): 1; preferably (0.8-1.5) 1; more preferably (1-1.2): 1.
Y represents yttrium cerium element. p represents the mole fraction of Y. P is more than or equal to 0.05 and less than or equal to 0.5; preferably, 0.1. Ltoreq. P.ltoreq.0.4. In some embodiments, 0.3. Ltoreq. P.ltoreq.0.5; preferably, 0.4. Ltoreq. P.ltoreq.0.45. In other embodiments, 0.1. Ltoreq. P.ltoreq.0.3; more preferably, 0.1. Ltoreq. P.ltoreq.0.2. The appropriate amount of Y for replacing Ca can improve the capacity retention rate of the hydrogen storage alloy after being recycled, and the hydrogen storage alloy has higher hydrogen absorption amount.
Ca represents calcium element. q represents the molar fraction of Ca. m + n + p + q =1. Q is more than or equal to 0.1 and less than or equal to 0.4; preferably, 0.2. Ltoreq. Q.ltoreq.0.3; more preferably, 0.2. Ltoreq. Q.ltoreq.0.23. This contributes to improvement in capacity retention and hydrogen absorption after recycling of the hydrogen occluding alloy.
Ni represents a nickel element. α represents a molar fraction of Ni. Alpha is more than or equal to 4.6 and less than or equal to 4.95; preferably, 4.7. Ltoreq. A.ltoreq.4.9; more preferably, 4.8. Ltoreq. A.ltoreq.4.9. Too low a content of nickel lowers the maximum hydrogen absorption amount of the hydrogen absorbing alloy and the capacity retention rate after recycling.
Mn represents a manganese element. Beta represents the molar fraction of Mn. Beta is more than or equal to 0.05 and less than or equal to 0.4; preferably, 0.1. Ltoreq. Beta.ltoreq.0.3; more preferably, 0.1. Ltoreq. Beta. Ltoreq.0.2. Mn can increase the hydrogen absorption amount and the capacity retention rate after recycling of the hydrogen storage alloy, but too high Mn content results in a decrease in the hydrogen absorption amount and the capacity retention rate.
Q is selected from one or more of Cu, sn, V, ti, zr, cr, zn, mo and Si; preferably, Q is selected from one or more of Cu, V, ti; more preferably, Q is selected from one of V or Ti.
γ represents the molar fraction of Q. Gamma is more than or equal to 0 and less than or equal to 0.2. In certain embodiments, γ =0. In other embodiments, 0.05. Ltoreq. Gamma. Ltoreq.0.15; preferably, 0.05. Ltoreq. Gamma. Ltoreq.0.1.
In the invention, 4.95 is less than or equal to alpha, beta and gamma is less than or equal to 5.2; preferably, 5 ≦ α + β + γ ≦ 5.1; more preferably, α + β + γ =5. This can improve the hydrogen absorption amount of the hydrogen absorbing alloy and the capacity retention rate after recycling.
Specific examples of yttrium-containing hydrogen storage alloys of the present invention include, but are not limited to, compositions represented by one of the following formulas:
La 0.4 Y 0.4 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Sm 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 V 0.1 ；
La 0.4 Ce 0.3 Y 0.1 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.3 Y 0.1 Ca 0.2 Ni 4.8 Mn 0.1 Ti 0.1 ；
La 0.3 Ce 0.2 Sm 0.1 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.2 Ce 0.2 Nd 0.2 Y 0.2 Ca 0.2 Ni 4.85 Mn 0.15 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 V 0.1 ；
La 0.4 Ce 0.1 Y 0.2 Ca 0.3 Ni 4.9 Mn 0.1 ；
La 0.3 Ce 0.25 Y 0.2 Ca 0.25 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.1 Y 0.3 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.2 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 Cu 0.1 ；
La 0.5 Ce 0.1 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.2 Ce 0.2 Y 0.3 Ca 0.3 Ni 4.7 Mn 0.3 。
the yttrium-containing hydrogen storage alloy is favorable for improving the hydrogen absorption amount and the capacity retention rate after recycling. The preferred technical scheme of the invention can ensure that the hydrogen storage alloy has lower hysteresis coefficient and hydride generation enthalpy.
The maximum hydrogen absorption amount of the rare earth hydrogen storage alloy is more than or equal to 1.63wt% at 40 ℃; preferably, the maximum hydrogen absorption amount is more than or equal to 1.65wt%; more preferably, the maximum hydrogen absorption amount is 1.67 to 1.69wt%. The capacity retention rate is more than or equal to 99.4 percent after 100 cycles; preferably, the capacity retention rate is more than or equal to 99.6 percent after 100 cycles; more preferably, the capacity retention rate is more than or equal to 99.7 percent after 100 cycles.
< preparation Process of Hydrogen storage alloy containing Yttrium >
The preparation process of the yttrium-containing hydrogen storage alloy comprises the following steps: smelting a metal raw material in an inert atmosphere to form a master alloy; and annealing the master alloy in an inert atmosphere to obtain the yttrium-containing hydrogen storage alloy.
The inert atmosphere may be selected from one or more of nitrogen, neon, argon. According to one embodiment of the invention, the inert atmosphere is an argon atmosphere.
The smelting temperature can be 1100-1600 ℃; preferably 1200 to 1500 ℃; more preferably 1300 to 1400 ℃. The smelting pressure can be 0.01-0.1 MPa; preferably 0.02 to 0.08MPa; more preferably 0.03 to 0.06MPa.
The annealing temperature can be 800-1200 ℃; preferably 900 to 1100 ℃; more preferably 1000 to 1100 ℃. The annealing pressure can be 0.01-0.1 MPa; preferably 0.02 to 0.08MPa; more preferably 0.03 to 0.06MPa. The annealing time can be 10-25 h; preferably 13 to 20 hours; more preferably 15 to 18 hours.
Examples 1 to 15 and comparative examples 1 to 2
The metal raw materials were formulated in accordance with the compositions of hydrogen occluding alloys shown in table 1. Polishing the rare earth metal in the metal raw material to obtain the treated rare earth metal. And polishing the metal Ca in the metal raw material to obtain the treated metal Ca.
The metal feedstock was placed in an alumina crucible. The metal raw material put in an alumina crucible is smelted under the conditions of 0.05MPa of pressure and 1400 ℃ of temperature in the Ar gas atmosphere to form the master alloy.
And (3) annealing the master alloy for 18h under the conditions of pressure of 0.06MPa and temperature of 1000 ℃ in Ar atmosphere to obtain the hydrogen storage alloy.
Examples of the experiments
And placing the obtained hydrogen storage alloy in a Sieverts device for testing to obtain a P-C-T curve of the hydrogen storage alloy at 40 ℃, obtaining the maximum hydrogen absorption amount, the hydrogen absorption platform pressure and the hydrogen discharge platform pressure according to the P-C-T curve, and calculating according to an equation to obtain the hydride generation enthalpy and the hysteresis coefficient.
Capacity retention on 100 cycles:
(1) The activated sample was subjected to dehydrogenation: vacuumizing for 1h at the normal temperature of 30 ℃ to ensure that the sample is completely dehydrogenated.
(2) Carrying out first hydrogen absorption circulation after sample dehydrogenation: filling hydrogen gas with a certain hydrogen pressure, recording the change of the hydrogen absorption amount of the sample along with the change of time until the hydrogen absorption amount is not changed, and recording the hydrogen absorption amount as the first hydrogen absorption amount C of the sample 1 。
(3) Repeating the steps 1 and 2 to complete multiple cycles of the alloy, and recording the hydrogen absorption C of each cycle n (n represents the number of cycles).
(4) The capacity retention ratio (S) of n cycles of the cycle was calculated according to the formula n )：S n ＝(C n /C 1 )×100％。
The properties of the hydrogen occluding alloy are shown in Table 1.
TABLE 1
The hydrogen occluding alloy of comparative example 3 does not contain yttrium on the hydrogen absorption side and does not contain Mn on the non-hydrogen absorption side, and both the maximum hydrogen absorption amount and the capacity retention rate at 100 cycles are lower than those of the yttrium-containing hydrogen occluding alloy of the present invention.
The hydrogen occluding alloy of comparative example 1 has a lower molar ratio of the element on the non-hydrogen-absorption side to the element on the hydrogen-absorption side, and the maximum hydrogen absorption amount and capacity retention rate after 100 cycles are both lower than those of example 4, and the enthalpy of hydride formation and hysteresis coefficient are increased.
The hydrogen occluding alloy of comparative example 2 has a reduced maximum hydrogen absorption amount and a capacity retention rate at 100 cycles as compared with example 2, and has an increased enthalpy of hydride formation and a hysteresis coefficient. This indicates that too high a content of Mn results in deterioration of the above properties.
The present invention is not limited to the above-described embodiments, and any variations, modifications, and alterations that may occur to those skilled in the art may fall within the scope of the present invention without departing from the spirit of the present invention.
Claims (10)
1. An yttrium-containing hydrogen storage alloy having the composition shown below:
La m M n Y p Ca q Ni α Mn β Q γ (I)
wherein M is selected from one or more of Ce, pr, nd, sm and Eu; q is selected from one or more of Cu, sn, V, ti, zr, cr, zn, mo and Si;
wherein m is more than or equal to 0.1 and less than or equal to 0.6, n is more than or equal to 0 and less than or equal to 0.5, p is more than or equal to 0.05 and less than or equal to 0.5, q is more than or equal to 0.1 and less than or equal to 0.4, and m + n + p + q =1; alpha is more than or equal to 4.6 and less than or equal to 4.95, beta is more than or equal to 0.05 and less than or equal to 0.4, gamma is more than or equal to 0 and less than or equal to 0.2, and alpha, beta and gamma are more than or equal to 4.95 and less than or equal to 5.2;
wherein m, n, p, q, alpha, beta and gamma represent the mole fraction of each element respectively.
2. The yttrium-containing hydrogen storage alloy of claim 1, wherein M comprises one or more of Ce or Sm.
3. An yttrium-containing hydrogen storage alloy according to claim 1, wherein M is selected from one of the following elemental compositions:
(1)Ce；
(2)Sm；
(3) Ce and Sm;
(4) Ce and Nd.
4. An yttrium-containing hydrogen storage alloy according to claim 1, wherein 0.1. Ltoreq. N.ltoreq.0.4.
5. An yttrium-containing hydrogen storage alloy according to claim 1, wherein 0.2. Ltoreq. M.ltoreq.0.5.
6. The yttrium-containing hydrogen storage alloy according to claim 1, wherein p is 0.1. Ltoreq. P.ltoreq.0.4.
7. An yttrium-containing hydrogen storage alloy according to claim 1, wherein q is 0.15. Ltoreq. Q.ltoreq.0.3.
8. The yttrium-containing hydrogen storage alloy according to claim 1, wherein α is 4.7. Ltoreq. α.ltoreq.4.95, β is 0.08. Ltoreq. β.ltoreq.0.3, a + b=5.
9. The yttrium-containing hydrogen storage alloy of claim 1, wherein said yttrium-containing hydrogen storage alloy has a composition of one of:
La 0.4 Y 0.4 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Sm 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 V 0.1 ；
La 0.4 Ce 0.3 Y 0.1 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.3 Y 0.1 Ca 0.2 Ni 4.8 Mn 0.1 Ti 0.1 ；
La 0.3 Ce 0.2 Sm 0.1 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.2 Ce 0.2 Nd 0.2 Y 0.2 Ca 0.2 Ni 4.85 Mn 0.15 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 V 0.1 ；
La 0.4 Ce 0.1 Y 0.2 Ca 0.3 Ni 4.9 Mn 0.1 ；
La 0.3 Ce 0.25 Y 0.2 Ca 0.25 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.1 Y 0.3 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.2 ；
La 0.4 Ce 0.2 Y 0.2 Ca 0.2 Ni 4.8 Mn 0.1 Cu 0.1 ；
La 0.5 Ce 0.1 Y 0.2 Ca 0.2 Ni 4.9 Mn 0.1 ；
La 0.2 Ce 0.2 Y 0.3 Ca 0.3 Ni 4.7 Mn 0.3 。
10. process for the preparation of an yttrium containing hydrogen storage alloy according to any one of claims 1 to 9, comprising the steps of:
smelting a metal raw material in an inert atmosphere at the temperature of 1100-1600 ℃ and under the pressure of 0.01-0.1 MPa to form a master alloy; and (3) annealing the master alloy in an inert atmosphere under the conditions that the pressure is 0.01-0.1 MPa and the temperature is 800-1200 ℃ to obtain the yttrium-containing hydrogen storage alloy.
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