CN114941058B - High-purity Pr5Co19 type La-Y-Ni superlattice alloy and preparation method thereof - Google Patents
High-purity Pr5Co19 type La-Y-Ni superlattice alloy and preparation method thereof Download PDFInfo
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- C21—METALLURGY OF IRON
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Abstract
The invention discloses a high-purity Pr5Co19 type La-Y-Ni superlattice alloy, which is prepared from metals La, Y and Ni through smelting and heat treatment of La-Y-Ni alloy 5 Co 19 La-Y-Ni superlattice alloy of superlattice phase; the La-Y-Ni superlattice alloy comprises, by mass, 35.7-39.4% of La, 3.2-8.2% of Y, and 52.4-61.1% of Ni and other unavoidable impurities; pr in the La-Y-Ni superlattice alloy 5 Co 19 The mass content of the superlattice phase is 84.5-96.3%. The preparation method comprises the following steps: smelting 1, la-Y-Ni alloy; and (3) heat treatment of the 2, la-Y-Ni alloy. The invention has the following advantages: 1.La-Y-Ni superlattice alloy with Pr of high purity 5 Co 19 A superlattice phase; 2. the preparation method is simple to operate, and the prepared alloy has stable structure and uniform components.
Description
Technical Field
The invention relates to a high-purity Pr5Co19 type La-Y-Ni superlattice alloy and a preparation method thereof, belonging to the technical field of material research methods.
Background
AB 5 The La-Mg-Ni based hydrogen storage alloy is mainly due to good electrochemical performance, high capacity and environmental friendlinessTo be used as anode materials for nickel metal hydride (Ni-MH) batteries. To date AB 5 The maximum discharge capacity of the alloy is 350 mAh.g -1 Its theoretical limit has been reached. La-Mg-Ni based hydrogen storage alloys are very difficult to prepare because they contain Mg with high volatility. The magnesium-free superlattice La-Y-Ni-based hydrogen storage alloy has higher theoretical discharge capacity and is considered as a potential substitute material (-400 mAh.g) -1 ). La-Y-Ni alloys containing several superlattice structures, e.g. AB 3 、A 2 B 7 And A 5 B 19 Phase of the type consisting of [ AB 5 ]And [ A ] 2 B 4 ]Subunits are stacked differently along the c-axis in a ratio of 1:1, 2:1, and 3:1. [ A ] 2 B 4 ]The subunit has MgZn 2 Laves and MgCu 2 Two structures of Laves, leading to AB 3 A is a 2 B 7 Form A and A 5 B 19 The superlattice phase forms two structures, 2H and 3R.
The La-Y-Ni superlattice alloy is easy to generate hydrogen-induced amorphization in the charge-discharge cycle process, and the superlattice structure of the phase is destroyed, so that the discharge capacity of the alloy decays rapidly. Research shows that hydrogen atoms occupy [ A ] in the hydrogen absorption process 2 B 4 ]The gaps of the subunits undergo lattice strain after multiple charge and discharge cycles, so that the hydrogen is amorphized. The sequence of the occurrence of hydrogen induced amorphization from easy to difficult is: AB (AB) 2 >AB 3 >A 2 B 7 >A 5 B 19 。
A 5 B 19 [ AB ] of superlattice phase 5 ]/[A 2 B 4 ]Higher than AB 3 And A 2 B 7 The superlattice phase can reduce lattice strain of the alloy, improve the phase content of the alloy, slow down hydrogen-induced amorphization of the alloy in the charge and discharge processes, and has better cycle stability. As in prior document 1 (Investigations on AB 3 -,A 2 B 7 -and A 5 B 19 -type La-Y-Ni system hydrogen storage alloys[J]International journal of hydrogen energy,2017,42 (4): 2257-2264), research on La-Y-Ni series AB by Yan et al 3 、A 2 B 7 And A 5 B 19 Structure and properties of hydrogen storage alloy, A 2 B 7 And A 5 B 19 The maximum discharge capacity of the alloy electrode at 298K is 385.7 mAh.g respectively -1 And 362.1 mAh.g -1 . The literature results indicate that A 5 B 19 Alloy ratio A 2 B 7 And AB 5 The shape alloy has better cycle stability.
A in La-Y-Ni System 5 B 19 Pr exists in superlattice phase 5 Co 19 (2H) and Ce 5 Co 19 Two structures of the type (3R) show Pr in the current research 5 Co 19 The structure has a specific Ce 5 Co 19 The profile structure has better stability and higher capacity. As in prior document 2 (Effect of Y element on cyclic stability of A 2 B 7 -type La-Y-Ni-based hydrogen storage alloy[J]International Journal of Hydrogen Energy,2019,44 (39): 22064-22073), liu et al explored the Y content versus La 3-x Y x Ni 9.7 Mn 0.5 Al 0.3 Influence of the cycling stability of the alloy. When x is less than 1.5, Y is substituted for La to prepare Ce 5 Co 19 And Pr 5 Co 19 La-Y-Ni alloy, pr coexisting in structure 5 Co 19 The superlattice phase increases with increasing Y content. Cycling stability and maximum discharge capacity with Pr 5 Co 19 The amount of the superlattice phase increases. The technical proposal successfully realizes that La is replaced by Y to improve Pr 5 Co 19 La (La) 5 Ni 19 The content of the phases. However, la-Y-Ni-based alloy inevitably undergoes phase transition upon cooling solidification, resulting in the coexistence of multiple phases in the alloy produced, and high purity Pr cannot be obtained 5 Co 19 A superlattice alloy.
The improvement of the preparation process can influence the solidification structure of the alloy, thereby improving Pr 5 Co 19 Purity of the superlattice phase. As in prior document 3 (study of La-Y-Ni based hydrogen storage alloy single-phase superlattice structure and capacity fading mechanism [ D ]]Preparation of AB by vacuum intermediate frequency induction melting at university of inner Mongolia 2021) He Xiangyang 5 Form A and A 2 B 4 Precursor, AB 5 Form A and A 2 B 4 And mixing and sintering the precursor powder according to the ratio of 3:1 for 5 hours to obtain the target single-phase alloy. AB (AB) 5 The precursor contains a small amount of AB 3 Impurity phase, A 2 B 4 The type precursor contains part of AB type hetero-phase, but the technical proposal has the technical problems that excessive La and Y elements in the alloy are segregated in smelting to generate hetero-phase, and the component deviation is larger. The burning loss ratio of La and Y elements can be adjusted to eliminate miscellaneous items in the precursor, but the prepared alloy is still Ce 5 Co 19 And Pr 5 Co 19 The mold structures coexist. According to the research of the applicant, the essential reason is that elements in La-Y-Ni alloy are segregated during cooling and solidification, so that the prepared alloy is subjected to phase transformation to generate other phases, and high-purity Pr is difficult to obtain 5 Co 19 A superlattice phase.
In order to solve the problem of reducing the segregation of elements in the hydrogen storage alloy, the alloy may be homogenized by annealing heat treatment. As in prior document 4 (rare earth and heat treatment for superlattice structure La-Y-Ni series A 5 B 19 Influence of Hydrogen storage and electrochemical Properties of alloys [ D]La prepared by arc melting, university of lanzhou rational worker, 2020) Yang Yang et al 0.4 Y 0.6 Ni 3.52 Mn 0.18 Al 0.1 The as-cast alloy was annealed at 1173K, 1223K, 1253K, 1273K, 1298K, 1323K, 1373K for 48 hours and furnace cooled to obtain La-Y-Ni superlattice alloy. A in alloy 5 B 19 The superlattice phases are Ce 5 Co 19 And Pr 5 Co 19 The two types of structures coexist. Pr in superlattice alloy prepared by annealing at different temperatures 5 Co 19 The superlattice phase mass content is 48.79% at most. Although this technique performs annealing heat treatment on the as-cast alloy, high purity Pr is not yet obtained 5 Co 19 La-Y-Ni superlattice alloy.
To sum up, pr 5 Co 19 La-Y-Ni superlattice alloy has excellent hydrogen storage properties, however, in the presently disclosed patent literature, la-Y-Ni based alloy is difficult to prepare high purity Pr 5 Co 19 The main technical problems are as follows:
1. element segregation occurs in the alloy ingot casting cooling process to cause phase change;
2. the existing preparation and heat treatment parameters can not obtain high-purity A 5 B 19 A superlattice phase.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a high-purity Pr5Co19 type La-Y-Ni superlattice alloy and a preparation method thereof.
The invention solves the problem of element segregation in the alloy by adjusting the alloy components and annealing heat treatment; combining with quenching heat treatment to obtain high-purity Pr 5 Co 19 La-Y-Ni superlattice alloy, and finally realizing uniform alloy components by simple process operation to obtain Pr with stable structure 5 Co 19 The purpose of the superlattice phase and effectively improving the content thereof is to provide a superlattice phase.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
a high-purity Pr5Co19 type La-Y-Ni superlattice alloy is prepared from La, Y and Ni through smelting and heat treatment to obtain Pr-contained alloy 5 Co 19 La-Y-Ni superlattice alloy of superlattice phase;
the La-Y-Ni superlattice alloy comprises, by mass, 35.7-39.4% of La, 3.2-8.2% of Y, and 52.4-61.1% of Ni and other unavoidable impurities;
pr in the La-Y-Ni superlattice alloy 5 Co 19 The mass content of the superlattice phase is 84.5-96.3%.
A preparation method of a high-purity Pr5Co19 type La-Y-Ni superlattice alloy comprises the following steps:
smelting La-Y-Ni alloy, namely weighing La, Y and Ni according to a certain mass percentage of the obtained alloy, smelting La, Y and Ni to obtain La-Y-Ni alloy melt, and cooling along with a furnace after the smelting process is finished to obtain La-Y-Ni alloy ingots;
the mass percent of the alloy in the step 1 is that the La content is 35.7-39.4 wt%, the Y content is 3.2-8.2 wt%, the Ni and other unavoidable impurities content is 52.4-61.1 wt%, and 5 wt% of La is added on the basis of target mass as burning loss compensation, and 5 wt% of Y is added on the basis of target mass as burning loss compensation;
the smelting method in the step 1 is arc smelting, and the specific arc smelting condition is that under the argon condition, the smelting current is 210-240A;
the smelting in the step 1 also comprises 3 links before smelting, during smelting and after smelting,
wherein, before smelting, vacuum is pumped until the vacuum degree reaches 3 multiplied by 10 -3 Pa, argon is filled until the pressure of the protective atmosphere is 0.05MPa, alloy melt is prevented from splashing, and then residual oxygen in a titanium ingot smelting furnace is smelted;
in the smelting process, after all the raw materials La, Y and Ni are melted into La-Y-Ni alloy melt, stirring the La-Y-Ni alloy melt through an electromagnetic coil for 1min;
after the smelting is finished, turning the obtained La-Y-Ni alloy ingot up and down, and repeating the smelting for 5 times;
step 2, performing heat treatment on the La-Y-Ni alloy, polishing the La-Y-Ni alloy ingot obtained in the step 1 by using sand paper to remove an oxide layer on the alloy surface, wrapping the La-Y-Ni alloy ingot by using tantalum foil, sealing the La-Y-Ni alloy ingot in a vacuum quartz tube, and performing annealing treatment and quenching treatment under certain conditions to obtain Pr 5 Co 19 La-Y-Ni superlattice alloy;
the annealing treatment condition in the step 2 is that the annealing temperature is 1000 ℃ and the annealing time is 24 hours;
and 2, quenching treatment conditions of the step are that after the annealing treatment is finished, the vacuum quartz tube is placed in an ice-water mixture for quenching treatment.
For the high purity Pr of the invention 5 Co 19 The La-Y-Ni superlattice alloy and the preparation method thereof are subjected to experimental detection, and the results are as follows:
XRD test results show that the alloy is prepared from Pr 5 Co 19 Superlattice phase (La, Y) 5 Ni 19 And Ce (Ce) 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 Composition is prepared.
XRD finishing results show that Pr in alloy 5 Co 19 Superlattice phase (La, Y) 5 Ni 19 The mass content of (2) is 84.5-96.3%, ce 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 The mass content of (3.7-15.5%).
SEM-BSE test results further showed that the alloy was composed of Pr 5 Co 19 Superlattice phase (La, Y) 5 Ni 19 And Ce (Ce) 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 Composition is prepared.
Test results show that the alloy is subjected to quenching heat treatment after annealing heat treatment at 1000 ℃ to obtain high-purity Pr 5 Co 19 La-Y-Ni superlattice alloy.
The test results show that compared with the prior art, the invention has the following advantages:
1. the La-Y-Ni superlattice alloy provided by the invention has Pr with high purity 5 Co 19 A superlattice phase;
2. the invention provides high purity Pr 5 Co 19 The preparation method of the La-Y-Ni superlattice alloy is simple to operate, and the prepared alloy has stable structure and uniform components.
Drawings
FIG. 1 is an XRD pattern and finishing result of La-Y-Ni alloy of example 1 of the present invention;
FIG. 2 is a graph showing the phase contents in examples and comparative examples according to the present invention;
FIG. 3 is an SEM-BSE image of La-Y-Ni alloy of example 1 of the present invention;
FIG. 4 is an XRD pattern and finishing result of the La-Y-Ni alloy of comparative example 1 of the present invention;
FIG. 5 is an XRD pattern and finishing result of La-Y-Ni alloy of example 2 of the present invention;
FIG. 6 shows XRD patterns and finishing results of the La-Y-Ni alloy of example 3 of the present invention.
Detailed Description
The present invention will now be described in further detail by way of examples, and not by way of limitation, with reference to the accompanying drawings.
Illustratively, the phases involved in the present invention include: pr (Pr) 5 Co 19 Superlattice phase (La, Y) 5 Ni 19 、Ce 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 And YNi 2 Wherein Pr is for convenience of explanation 5 Co 19 Superlattice phase (La, Y) 5 Ni 19 Abbreviated as phase I.
Example 1
A preparation method of a high-purity Pr5Co19 type La-Y-Ni superlattice alloy comprises the following steps:
smelting La-Y-Ni alloy, namely firstly, taking the obtained alloy with the mass percent of 35.7wt.% La, 3.2wt.% Y and 61.1wt.% Ni and other unavoidable impurities as required, adding 5wt.% La as a burning loss compensation on the basis of target mass, adding 5wt.% Y as a burning loss compensation on the basis of target mass, weighing La, Y and Ni, wherein the purities of the used raw materials are not lower than 99.99wt.%, and then carrying out arc smelting on La, Y and Ni with smelting current of 240A under argon condition to obtain La-Y-Ni alloy melt, and cooling along with a furnace to obtain La-Y-Ni alloy ingot after the smelting process is finished;
before smelting, vacuumizing until the vacuum degree reaches 3X 10 -3 Pa, argon is filled until the pressure of the protective atmosphere is 0.05MPa, alloy melt is prevented from splashing, and then residual oxygen in a titanium ingot smelting furnace is smelted; in the smelting process, after all the raw materials La, Y and Ni are melted into La-Y-Ni alloy melt, stirring the La-Y-Ni alloy melt through an electromagnetic coil for 1min; after the smelting is finished, turning the obtained La-Y-Ni alloy ingot up and down, and repeating the smelting for 5 times;
step 2, performing heat treatment on the La-Y-Ni alloy, polishing the La-Y-Ni alloy ingot obtained in the step 1 by using sand paper to remove an oxide layer on the alloy surface, wrapping the La-Y-Ni alloy ingot by using a tantalum foil, sealing the alloy in a vacuum quartz tube, performing annealing treatment under the condition that the annealing temperature is 1000 ℃ and the annealing time is 24 hours, and after the annealing treatment is finished, placing the vacuum quartz tube in an ice-water mixture for quenching treatment to obtain Pr 5 Co 19 La-Y-Ni superlattice alloy La-3.2Y-61.1Ni-1000, abbreviated as alloy 1-1.
To demonstrate the phase composition of alloy 1-1, XRD testing was performed, and to further confirm the content of the phase, the XRD test results were refined. XRD testing and finishing results are shown in FIG. 1, alloy 1-1 consisting of phase I and Ce 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 The composition, the content of phase, is shown in FIG. 2 and Table 1, the mass content of phase I is 96.3% (La, Y) 2 Ni 7 The mass content of the phase was 3.7%.
TABLE 1 phase composition and phase content of La-Y-Ni alloy
To further confirm the phase composition of alloy 1-1, SEM-BSE tests were performed. The test results are shown in FIG. 3, in which the dark gray region is phase I and the light gray region is (La, Y) 2 Ni 7 And (3) phase (C). Test results show that alloy 1-1 obtains high purity Pr after annealing heat treatment at 1000 DEG C 5 Co 19 La-Y-Ni superlattice alloy.
To demonstrate the effect of heat treatment temperature on the phase composition of La-Y-Ni alloy, comparative example 1, a method for producing La-Y-Ni alloy having an annealing temperature of 875℃was provided.
Comparative example 1
A method for producing an La-Y-Ni alloy having an annealing temperature of 875 ℃ was the same as in example 1 except that the steps not specifically described were: the annealing temperature in the step 2 is 875 ℃, and La-3.2Y-61.1Ni-875 is simply called alloy 2.
To confirm the phase composition of alloy 2, XRD testing was performed, and to further confirm the content of the phase, the XRD test results were refined. XRD testing and finishing results are shown in FIG. 4, alloy 2 is composed of Ce 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 And YNi 2 Phase composition; the phase content is shown in FIG. 2 and Table 1, (La, Y) 2 Ni 7 The mass content of the phase is 76.1％，YNi 2 The mass content of the phase was 23.9%.
As can be seen from the above test results, pr could not be obtained after annealing heat treatment of alloy 2 at 875 ℃ 5 Co 19 A superlattice phase.
Example 2
A method for preparing a high purity Pr5Co19 type La-Y-Ni superlattice alloy, the procedure not specifically described is the same as in example 1, except that: the alloy in the step 1 is prepared by the following steps of 36.5wt.% of La, 4.5wt.% of Y and 59.0wt.% of Ni and other unavoidable impurities, wherein La-4.5Y-59.0Ni-1000 is simply referred to as alloy 1-2.
To demonstrate the phase composition of alloys 1-2, XRD testing was performed, and to further confirm the content of the phases, the XRD test results were refined. XRD testing and finishing results are shown in FIG. 5, where alloys 1-2 consist of phase I and Ce 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 Composition; the content of the phase is shown in FIG. 2 and Table 1, and the mass content of the phase I is 87.8% (La, Y) 2 Ni 7 The mass content of the phase was 12.2%.
Test results show that after annealing heat treatment of the alloy 1-2 at 1000 ℃, high purity Pr can be obtained 5 Co 19 La-Y-Ni superlattice alloy and no Ce generation 5 Co 19 A superlattice phase.
Example 3
A method for preparing a high purity Pr5Co19 type La-Y-Ni superlattice alloy, the procedure not specifically described is the same as in example 1, except that: the alloy in the step 1 is prepared by the following steps of 36.3wt.% of La, 5.5wt.% of Y and 58.2wt.% of Ni and other unavoidable impurities, wherein La-5.5Y-58.2Ni-1000 is simply referred to as alloy 1-3.
To demonstrate the phase composition of alloys 1-3, XRD testing was performed, and to further confirm the content of the phases, the XRD test results were refined. XRD testing and finishing results are shown in FIG. 6, where alloys 1-3 consist of phase I and Ce 2 Ni 7 Superlattice phase (La, Y) 2 Ni 7 Composition; phase contentThe amounts are shown in FIG. 2 and Table 1, the mass content of phase I was 84.5% (La, Y) 2 Ni 7 The mass content of the phase was 15.5%.
Test results show that after annealing heat treatment of the alloy 1-3 at 1000 ℃, high purity Pr can be obtained 5 Co 19 La-Y-Ni superlattice alloy and no Ce generation 5 Co 19 A superlattice phase.
Claims (2)
1. A high-purity Pr5Co19 type La-Y-Ni superlattice alloy is characterized in that: smelting and heat treating La-Y-Ni alloy to obtain Pr-containing alloy with La, Y and Ni as material 5 Co 19 La-Y-Ni superlattice alloy of superlattice phase;
the La-Y-Ni superlattice alloy comprises, by mass, 35.7-39.4% of La, 3.2-8.2% of Y, and 52.4-61.1% of Ni and other unavoidable impurities;
pr in the La-Y-Ni superlattice alloy 5 Co 19 The mass content of the superlattice phase is 84.5-96.3%.
2. The preparation method of the high-purity Pr5Co19 type La-Y-Ni superlattice alloy is characterized by comprising the following steps of:
smelting La-Y-Ni alloy, namely weighing La, Y and Ni according to a certain mass percentage of the obtained alloy, smelting La, Y and Ni to obtain La-Y-Ni alloy melt, and cooling along with a furnace after the smelting process is finished to obtain La-Y-Ni alloy ingots;
the mass percent of the alloy in the step 1 is that the La content is 35.7-39.4 wt%, the Y content is 3.2-8.2 wt%, the Ni and other unavoidable impurities content is 52.4-61.1 wt%, and 5 wt% of La is added on the basis of target mass as burning loss compensation, and 5 wt% of Y is added on the basis of target mass as burning loss compensation;
the smelting method in the step 1 is arc smelting, and the specific arc smelting condition is that under the argon condition, the smelting current is 210-240A;
the smelting of the step 1 is carried outBefore smelting, the smelting process and 3 links after smelting are completed, wherein vacuum is pumped until the vacuum degree reaches 3 multiplied by 10 before smelting -3 Pa, argon is filled until the pressure of the protective atmosphere is 0.05MPa, alloy melt is prevented from splashing, and then residual oxygen in a titanium ingot smelting furnace is smelted; in the smelting process, after all the raw materials La, Y and Ni are melted into La-Y-Ni alloy melt, stirring the La-Y-Ni alloy melt through an electromagnetic coil for 1min; after the smelting is finished, turning the obtained La-Y-Ni alloy ingot up and down, and repeating the smelting for 5 times;
step 2, performing heat treatment on the La-Y-Ni alloy, namely polishing the La-Y-Ni alloy ingot obtained in the step 1 by using sand paper to remove an oxide layer on the surface of the alloy, wrapping the alloy with a tantalum foil, sealing the alloy in a vacuum quartz tube, and performing annealing treatment and quenching treatment under certain conditions to obtain Pr5Co19 type La-Y-Ni superlattice alloy;
the annealing treatment condition in the step 2 is that the annealing temperature is 1000 ℃ and the annealing time is 24 hours;
and 2, quenching treatment conditions of the step are that after the annealing treatment is finished, the vacuum quartz tube is placed in an ice-water mixture for quenching treatment.
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