CN107201457A - A kind of preparation method of Gd2Co7 types Nd-Mg-Ni systems single-phase alloy - Google Patents

A kind of preparation method of Gd2Co7 types Nd-Mg-Ni systems single-phase alloy Download PDF

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CN107201457A
CN107201457A CN201710522126.9A CN201710522126A CN107201457A CN 107201457 A CN107201457 A CN 107201457A CN 201710522126 A CN201710522126 A CN 201710522126A CN 107201457 A CN107201457 A CN 107201457A
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韩树民
贾泽茹
张璐
赵雨萌
曹娟
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/24—Alkaline accumulators
    • H01M10/30—Nickel accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/383—Hydrogen absorbing alloys
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

A kind of Gd2Co7The preparation method of type Nd-Mg-Ni systems single-phase alloy, its predecessor Nd for mainly obtaining induction melting0.8Mg0.2Ni2.7And Mg2Ni ingot castings grind to form the powder that granularity is less than 400 mesh, according to nickel powder：Nd0.8Mg0.2Ni2.7：Mg2Ni mol ratio is 1:0.38~0.42:0.01~0.02 ratio, they are well mixed；The cold moudling under 5~5.5MPa pressure, carries out the powder sintered processing of substep in tube furnace：950 DEG C are warming up to from room temperature by five times, 850 DEG C, 1 DEG C/min of rate of temperature fall are finally cooled to from 950 DEG C；Sintering procedure terminates, and alloy is cooled to room temperature with furnace temperature.Present device is simple, technological operation is simple, conditional stability, and alloying component is easily controlled, and sintering obtained alloy has preferable structural stability and comprehensive electrochemical.

Description

A kind of preparation method of Gd2Co7 types Nd-Mg-Ni systems single-phase alloy
Technical field：
The invention belongs to field of material technology, more particularly to a kind of preparation method of hydrogen-storage alloy.
Background technology：
Metal-hydrogen nickel battery (Ni/MH) is a kind of novel high-capacity secondary cell, can be widely applied to portable electric The fields such as sub- equipment, electric car, hybrid electric.It is compared with development at present is than relatively rapid lithium ion (Li) battery, tool Have the advantages that safety non-pollution, memory-less effect and anti-over-charging/discharge capability are strong.In Ni/MH batteries, negative material is influence One of topmost factor of battery physical and chemical performance.Ni/MH cell negative electrode materials commercially use at present are mainly AB5 Type rare earth based hydrogen storage alloy, but such alloy is limited by crystal structure, intrinsic hydrogen storage content is relatively low, and electrochemistry capacitance is Through reaching 300-330mAh/g, it is difficult to meet the demand that battery performance further develops again.Therefore, new negative pole is researched and developed Material is significant.
The beginning of this century starts the RE-Mg-Ni series hydrogen storage alloys being widely studied, with different from AB5Type alloy it is special Superlattice structure, each of which structure cell is all by [RENi5] and [REMgNi4] subunit forms along c-axis direction periodicity stacking , and different [RENi5]/[REMgNi4] subunit ratio stacking is into different structures.Specifically, subunit is worked as [RENi5]/[REMgNi4] ratio be 1:1、2:1 and 3:When 1, AB can be formed3Type, A2B7Type and A5B19Type structure, and every kind of knot Structure is again according to the [REMgNi of its various configuration included4] subunit, it is divided into 2H (CeNi3、Ce2Ni7、Pr5Co19) and 3R (PuNi3、Gd2Co7、Ce5Co19) two kinds of configurations.Wherein, the characteristics of La-Mg-Ni series hydrogen storage alloys have high power capacity, it is considered to be Preferable cell negative electrode material, but the cyclical stability of such alloy is poor.Compared with La elements, the atomic radius of Nd elements Smaller, chemism is relatively low, it is not easy to occurs oxidation and corrodes, and in alkaline electrolyte, can generate layer of oxide layer resistance The only further oxidation and corrosion of alloy, therefore compared to La-Mg-Ni systems alloy, Nd-Mg-Ni systems alloy is shown preferably Cyclical stability.
Du in 2016 et al. [W.K.Du, L.Zhang, Y.Li, et al.J.Electrochem.Soc., 2016,163 (7):A1474-A1483] method that is made annealing treatment with subregion is prepared for PuNi3Type Nd-Mg-Ni systems single-phase alloy, and point out with PuNi3Type La2MgNi9Single-phase alloy is compared, Nd2MgNi9Single-phase alloy shows excellent cycle life, its 100 weeks circulation Stability is 92%.Research shows, with AB3Type alloy is compared, A2B7The subunit of type alloy Volume Changes during hydrogen is put in suction Difference reduction, structural stability is improved, therefore A2B7Type alloy shows higher cycle life.
K.Young et al. [K.Young, T.Ouchi, B.Huang.J.Power Sources, 2014,248 (7):147- 153] obtain a series of with Ce2Ni7It is mutually (Nd, Mg, Zr) (Ni, Al, Co) alloy of principal phase, and it was found that with alloy The reduction of other phase contents, the chemical property of alloy constantly improves, especially cyclical stability, and this explanation prepares single-phase alloy Performance for improvement alloy is significant.And Zhang et al. [Q.A.Zhang, B.Zhao, M.H.Fang, et al.Inorg.Chem.,2012,51(5):2976-2983] point out, for the less Nd elements of atomic radius, occur peritectic reaction When be more likely to generation 3R (PuNi3、Gd2Co7、Ce5Co19) type structure, so for Nd-Mg-Ni systems alloy, 3R configurations Gd2Co7Structure is more stablized, but does not have document report Gd still at present2Co7The preparation method and electrification of type Nd-Mg-Ni systems alloy Performance is learned, therefore, Gd is prepared2Co7Structural stability and chemical property of the single-phase Nd-Mg-Ni alloys of type for research alloy It is significant.
The content of the invention：
It is an object of the invention to provide a kind of method is simple and reliable, the easily operated control of technique, with excellent electrochemistry The Gd of cyclical stability2Co7The preparation method of type Nd-Mg-Ni systems single-phase alloy.
The method of the present invention is comprised the following steps that：
(1) Nd obtained with induction melting0.8Mg0.2Ni2.7And Mg2Ni alloy cast ingots are protected as predecessor in argon gas atmosphere The lower mechanical crushing of shield is less than 400 mesh powders into diameter, then according to nickel powder：Nd0.8Mg0.2Ni2.7：Mg2Ni mol ratio is 1: 0.38~0.42:0.01~0.02 ratio, they are well mixed；
(2) by mixture cold moudling under 5~5.5MPa pressure of step (1), it is put into closed in stainless steel sintering tank Obturage；
(3) the sintering tank of step (2) good seal is put into tube furnace, be sintered under 0~0.01MPa argon atmospheres Processing, sintering procedure is as follows：First, 250 DEG C are risen to from room temperature, heating rate is 5 DEG C/min, constant temperature 2h；Then risen from 250 DEG C Temperature is to 500 DEG C, heating rate 5 DEG C/min, constant temperature 2h；800 DEG C, 10 DEG C/min of heating rate, constant temperature are warming up to from 500 DEG C again 1h；Then proceed to be warming up to 900 DEG C, heating rate 1 DEG C/min, constant temperature 48h from 800 DEG C；950 DEG C, liter are warming up to from 900 DEG C again Warm 1 DEG C/min of speed, constant temperature 60h；850 DEG C, 1 DEG C/min of rate of temperature fall are finally cooled to from 950 DEG C；Sintering procedure terminates, and closes Gold is cooled to room temperature with furnace temperature, you can obtain Gd2Co7Type Nd-Mg-Ni systems single-phase alloy, consisting of Nd0.78~ 0.82Mg0.22~0.18Ni3.46~3.5。
The present invention has the following advantages that compared with prior art：
(1) equipment is simple, technological operation is simple, conditional stability, and alloying component is easily controlled, being capable of controllable preparation spy Determine the alloy of phase structure.
(2) Nd-Mg-Ni systems alloy has Gd made from2Co7Type single-phase crystal-structure, and it is steady to show preferable structure Qualitative and comprehensive electrochemical.
Brief description of the drawings：
Fig. 1 is Gd prepared by the embodiment of the present invention 1,2 and 32Co7Type Nd-Mg-Ni are the Rietveld of single-phase hydrogen-storage alloy Fitted figure.
Fig. 2 is Gd prepared by the embodiment of the present invention 1,2 and 32Co7Type Nd-Mg-Ni system's single phase alloy electrode discharge capacities with Circulating cycle number graph of relation.
Fig. 3 is Gd prepared by the embodiment of the present invention 1,2 and 32Co7The high magnification of type Nd-Mg-Ni systems single phase alloy electrode is put Electric curve map.
Embodiment：
Embodiment 1
The Nd obtained with induction melting0.8Mg0.2Ni2.7And Mg2Ni alloy cast ingots are as predecessor, in argon gas atmosphere protection Lower mechanical crushing is less than 400 mesh powders into diameter, then according to nickel powder：Nd0.8Mg0.2Ni2.7：Mg2Ni mol ratio is 1: 0.38:0.01 ratio, they are well mixed；By said mixture cold moudling under 5MPa pressure, stainless steel burning is put into It is closed in knot tank to obturage；The sintering tank of good seal is put into tube furnace, is sintered under 0.01MPa argon atmospheres, Sintering procedure is as follows：First, 250 DEG C are risen to from room temperature, heating rate is 5 DEG C/min, constant temperature 2h；Then it is warming up to from 250 DEG C 500 DEG C, heating rate 5 DEG C/min, constant temperature 2h；800 DEG C, heating rate 10 DEG C/min, constant temperature 1h are warming up to from 500 DEG C again；So After continue to be warming up to 900 DEG C, heating rate 1 DEG C/min, constant temperature 48h from 800 DEG C；950 DEG C, heating speed are warming up to from 900 DEG C again Rate 1 DEG C/min, constant temperature 60h；850 DEG C, 1 DEG C/min of rate of temperature fall are finally cooled to from 950 DEG C；Sintering procedure terminates, alloy with Furnace temperature is cooled to room temperature, you can obtain Gd2Co7Type Nd-Mg-Ni systems single-phase alloy, alloy composition is Nd0.82Mg0.18Ni3.5, its X Shown in x ray diffraction refine collection of illustrative plates such as Fig. 1 (a).
The alloy of above-mentioned sintering is ground off into surface oxide layer, mechanical crushing takes diameter to be less than 200 mesh powders and carbonyl nickel Powder is according to 1:Nickel-hydrogen battery negative pole piece is made in 5 ratio, with the hickelous nydroxide (Ni (OH) of sintering2/ NiOOH) positive pole is done, 6mol L-1The KOH aqueous solution two electrode half-cell systems are made for electrolyte, utilize DC-5 cell tester beta alloy electrodes Chemical property.The Gd prepared2Co7The chemical property of type Nd-Mg-Ni systems single phase alloy electrode is as shown in Fig. 2 alloy Electrode can be activated completely through three charge and discharge cycles, and maximum discharge capacity is 340mAh/g, by 100 circle charge and discharge cycles Afterwards, capability retention is 74%；High-rate discharge ability is as shown in figure 3, alloy electrode is transferred in 1200mA/g current density Capacitance is 180mAh/g, is 150mAh/g, HRD in 1500mA/g current density discharge capacity1200And HRD1500Respectively 66% and 55%.
Embodiment 2
The Nd obtained with induction melting0.8Mg0.2Ni2.7And Mg2Ni alloy cast ingots are as predecessor, in argon gas atmosphere protection Lower mechanical crushing is less than 400 mesh powders into diameter, then according to nickel powder：Nd0.8Mg0.2Ni2.7：Mg2Ni mol ratio is 1: 0.4:0.015 ratio, they are well mixed；By said mixture cold moudling under 5.3MPa pressure, stainless steel is put into It is closed in sintering tank to obturage；The sintering tank of good seal is put into tube furnace, place is sintered under 0.01MPa argon atmospheres Reason, sintering procedure is as follows：First, 250 DEG C are risen to from room temperature, heating rate is 5 DEG C/min, constant temperature 2h；Then from 250 DEG C of heatings To 500 DEG C, heating rate 5 DEG C/min, constant temperature 2h；800 DEG C, heating rate 10 DEG C/min, constant temperature 1h are warming up to from 500 DEG C again； Then proceed to be warming up to 900 DEG C, heating rate 1 DEG C/min, constant temperature 48h from 800 DEG C；950 DEG C, heating are warming up to from 900 DEG C again Speed 1 DEG C/min, constant temperature 60h；850 DEG C, 1 DEG C/min of rate of temperature fall are finally cooled to from 950 DEG C；Sintering procedure terminates, alloy Room temperature is cooled to furnace temperature, you can obtain Gd2Co7Type Nd-Mg-Ni systems single-phase alloy, alloy composition is Nd0.80Mg0.2Ni3.46, Shown in its X-ray diffraction refine collection of illustrative plates such as Fig. 1 (b).
According to the method for embodiment 1, alloy electrode is made in alloy, its chemical property is tested, as a result as shown in Fig. 2 The Gd that the example is prepared2Co7Type Nd-Mg-Ni systems single phase alloy electrode can be activated completely by two charge and discharge cycles, most Big discharge capacity is 342mAh/g, and after 100 circle charge and discharge cycles, capability retention is 74%；High-rate discharge ability is such as Shown in Fig. 3, its HRD1200And HRD1500Respectively 64% and 53%.
Embodiment 3
The Nd obtained with induction melting0.8Mg0.2Ni2.7And Mg2Ni alloy cast ingots are as predecessor, in argon gas atmosphere protection Lower mechanical crushing is less than 400 mesh powders into diameter, then according to nickel powder：Nd0.8Mg0.2Ni2.7：Mg2Ni mol ratio is 1: 0.42:0.02 ratio, they are well mixed；By said mixture cold moudling under 5.5MPa pressure, stainless steel is put into It is closed in sintering tank to obturage.The sintering tank of good seal is put into tube furnace, place is sintered under 0.01MPa argon atmospheres Reason, sintering procedure is as follows：First, 250 DEG C are risen to from room temperature, heating rate is 5 DEG C/min, constant temperature 2h；Then from 250 DEG C of heatings To 500 DEG C, heating rate 5 DEG C/min, constant temperature 2h；800 DEG C, heating rate 10 DEG C/min, constant temperature 1h are warming up to from 500 DEG C again； Then proceed to be warming up to 900 DEG C, heating rate 1 DEG C/min, constant temperature 48h from 800 DEG C；950 DEG C, heating are warming up to from 900 DEG C again Speed 1 DEG C/min, constant temperature 60h；850 DEG C, 1 DEG C/min of rate of temperature fall are finally cooled to from 950 DEG C；Sintering procedure terminates, alloy Room temperature is cooled to furnace temperature, you can obtain Gd2Co7Type Nd-Mg-Ni systems single-phase alloy, alloy composition is Nd0.78Mg0.22Ni3.48, Shown in its X-ray diffraction refine collection of illustrative plates such as Fig. 1 (c).
According to the method for embodiment 1, alloy electrode is made in alloy, its chemical property is tested, as a result as shown in Fig. 2 The Gd that the example is prepared2Co7Type Nd-Mg-Ni systems single phase alloy electrode can be activated completely by two charge and discharge cycles, most Big discharge capacity is 345mAh/g, and after 100 circle charge and discharge cycles, capability retention is 74%；High-rate discharge ability is such as Shown in Fig. 3, its HRD1200And HRD1500Respectively 65.3% and 57.9%.

Claims (1)

1. a kind of Gd2Co7The preparation method of type Nd-Mg-Ni systems single-phase alloy, it is characterised in that：It is comprised the following steps that：
(1) Nd obtained with induction melting0.8Mg0.2Ni2.7And Mg2Ni alloy cast ingots are as predecessor, under argon gas atmosphere protection Mechanical crushing is less than 400 mesh powders into diameter, then according to nickel powder：Nd0.8Mg0.2Ni2.7：Mg2Ni mol ratio is 1:0.38 ~0.42:0.01~0.02 ratio, they are well mixed；
(2) by mixture cold moudling under 5~5.5MPa pressure of step (1), it is put into closed in stainless steel sintering tank obturage；
(3) the sintering tank of step (2) good seal is put into tube furnace, place is sintered under 0~0.01MPa argon atmospheres Reason, sintering procedure is as follows：First, 250 DEG C are risen to from room temperature, heating rate is 5 DEG C/min, constant temperature 2h；Then from 250 DEG C of heatings To 500 DEG C, heating rate 5 DEG C/min, constant temperature 2h；800 DEG C, heating rate 10 DEG C/min, constant temperature 1h are warming up to from 500 DEG C again； Then proceed to be warming up to 900 DEG C, heating rate 1 DEG C/min, constant temperature 48h from 800 DEG C；950 DEG C, heating are warming up to from 900 DEG C again Speed 1 DEG C/min, constant temperature 60h；850 DEG C, 1 DEG C/min of rate of temperature fall are finally cooled to from 950 DEG C；Sintering procedure terminates, alloy Room temperature is cooled to furnace temperature, you can obtain Gd2Co7Type Nd-Mg-Ni systems single-phase alloy, consisting of Nd0.78~0.82Mg0.22~ 0.18Ni3.46~3.5。
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Cited By (2)

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CN116219228A (en) * 2023-03-03 2023-06-06 包头中科轩达新能源科技有限公司 A kind of (Gd, mg) 2 Ni 7 Preparation method of superlattice hydrogen storage alloy

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