CN113122884B - Preparation method of rare earth intermediate alloy for hydrogen storage alloy - Google Patents
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- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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Abstract
The invention relates to a method for preparing a rare earth intermediate alloy for hydrogen storage alloy, wherein the alloy simultaneously contains rare earth elements and nickel elements; the mass percentage of the rare earth element and the nickel element is (40-90) to (10-60). The method comprises the steps of taking a graphite crucible as an electrolytic bath, taking a graphite block as an anode, taking a nickel rod as a consumable cathode, adding one or more rare earth oxides into a binary or multielement electrolyte system consisting of rare earth fluoride and alkali metal or alkaline earth metal fluoride, introducing direct current, discharging rare earth cations at the nickel cathode and carrying out alloying, dripping and gathering alloy generated by reaction in a receiver of the electrolytic bath, taking out and casting to obtain the rare earth intermediate alloy for the hydrogen storage alloy. When the hydrogen storage alloy containing rare earth and nickel elements is prepared, the low-cost high-quality intermediate alloy is used for replacing expensive simple substance rare earth metal as a raw material, so that the cost of the hydrogen storage alloy can be obviously reduced, and the market application of the hydrogen storage alloy is facilitated.
Description
The application is a divisional application with the application number of 201611134246.3 and the invention name of rare earth intermediate alloy for hydrogen storage alloy and a preparation method thereof, which is filed as 20161210 by the applicant at the filing date.
Technical Field
The invention relates to a rare earth intermediate alloy for hydrogen storage alloy and a preparation method thereof, in particular to a binary and multi-element rare earth intermediate alloy for hydrogen storage alloy and a preparation method thereof.
Background
Hydrogen storage alloys are green functional materials that react with hydrogen to form metal hydrides and release hydrogen reversibly under appropriate conditions, and their most successful application is as the negative electrode material of nickel-metal hydride (Ni-MH) batteries. Hydrogen storage alloys which have been commercially used today are mainly AB 5 Type rare earth hydrogen storage alloy Mm (NiCoMnAl) 5 (Mm is a misch metal). AB 5 The capacity (340 mAh/g) of the type hydrogen storage alloy has beenIt has been quite difficult to further improve upon approaching its theoretical value (372 mAh/g), and therefore, the development of hydrogen storage alloys with higher capacity is a hot spot of current hydrogen storage alloy research.
To improve AB 5 The research workers also carry out a great deal of element substitution research work on the comprehensive properties of the hydrogen storage alloys such as the type or La-Mg-Ni alloy and the like. China has abundant yttrium (Y) resources, and the utilization of yttrium element to improve the performance of hydrogen storage alloy has important significance, for example Luo Yongchun and other people research La 3-x Y x MgNi 14 (x = 0-2) phase structure and electrochemical performance of hydrogen storage alloys (Luo Yongchun, chen Jiangping, zhang Faliang, yan Ruxu, kang Long, chen Jianhong, proceedings of the university of Ringtech, lanzhou, 2006, 32 (4): 20-24) have led to several valuable conclusions. The inventor discovers that the rare earth-yttrium-nickel hydrogen storage alloy has better hydrogen storage performance when researching novel yttrium-containing hydrogen storage alloy, and the discharge capacity of the rare earth-yttrium-nickel hydrogen storage alloy can reach more than 380mAh/g and exceeds AB 5 The alloy has the advantages of theoretical discharge capacity, long cycle life, no volatile element contained in the alloy, and relatively simple preparation, and is expected to become a new generation of high-capacity hydrogen storage alloy.
Although the hydrogen storage alloy containing yttrium has better hydrogen storage performance, the cost is higher, mainly because the main element yttrium in the prior alloy is prepared by a metallothermic reduction method, and the preparation method has long process flow and adopts active metal calcium as a reducing agent, so the production cost is high, and the yttrium price is high.
Disclosure of Invention
The invention aims to overcome the problem of higher cost of hydrogen storage alloy containing rare earth and nickel when rare earth metal is used as a raw material, and provides a rare earth intermediate alloy for the hydrogen storage alloy simultaneously containing Rare Earth (RE) elements and nickel (Ni) elements and a preparation method thereof.
The technical scheme of the invention is as follows:
a rare earth intermediate alloy for hydrogen storage alloy is characterized in that: the alloy contains Rare Earth (RE) element and nickel (Ni) element at the same time; the mass percentage of the rare earth elements and the nickel elements is RE: ni = (40-90): (10-60).
The rare earth element is one or more of scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium and lutetium.
The preparation method of the rare earth master alloy for the hydrogen storage alloy comprises the following steps: the method comprises the steps of taking a graphite crucible as an electrolytic bath, taking a graphite block as an anode, taking a nickel rod as a consumable cathode, adding one or more rare earth oxides into a binary or multielement electrolyte system consisting of rare earth fluoride and alkali metal or alkaline earth metal fluoride, introducing direct current, discharging rare earth cations at the nickel cathode and carrying out alloying, dripping and gathering alloy generated by reaction in a receiver of the electrolytic bath, taking out and casting to obtain the rare earth intermediate alloy for the hydrogen storage alloy.
The nickel cathode is a round bar, a square bar or a plate, and the number of the nickel cathodes is one or more.
The binary or multielement electrolyte composed of the rare earth fluoride and the alkali metal or alkaline earth metal fluoride, wherein the mass fraction of the rare earth fluoride is 60-97%.
The electrolysis temperature in the electrolysis process is 900-1200 ℃.
The anode current density in the electrolysis process is 0.3-3.0A/cm 2 The cathode current density is 5-25A/cm 2 。
The invention has the advantages that: the rare earth intermediate alloy is adopted to prepare the hydrogen storage alloy, so that expensive simple substance rare earth metal is not used as a raw material when the hydrogen storage alloy containing rare earth and nickel elements is prepared, the cost of the hydrogen storage alloy containing rare earth and nickel elements can be obviously reduced, and the hydrogen storage alloy containing rare earth and nickel elements is beneficial to market application.
Detailed Description
A rare earth intermediate alloy for hydrogen storage alloy contains Rare Earth (RE) element and nickel (Ni) element; the mass percentage of the rare earth elements and the nickel elements is RE: ni = (40-90): (10-60).
The rare earth elements are: one or more of scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium and lutetium.
The alloy of the invention is prepared by an electrolytic method, and the basic steps are as follows:
(1) Determining proper electrolyte composition according to the rare earth intermediate alloy for the hydrogen storage alloy to be prepared;
(2) Determining reasonable anode and cathode current density according to the prepared rare earth intermediate alloy for the hydrogen storage alloy and the scale of the electrolytic cell;
(3) Installing a cathode and an anode, filling the electrolyte which is distributed according to a certain distribution, and short-circuiting the cathode and the anode to generate heat to melt the electrolyte;
(4) Adjusting the temperature of the electrolytic cell to a proper temperature, adding rare earth oxide, and starting normal electrolysis;
(5) In the electrolytic process, oxide raw materials are added at a certain feeding speed, the cathode is adjusted down at certain intervals, and the current and the voltage are kept stable;
(6) After electrolysis for a period of time, discharging, casting into ingots, cooling and demoulding to obtain the rare earth intermediate alloy for the hydrogen storage alloy.
The following examples are provided to further illustrate the details of the present invention and its embodiments.
Example 1: the molten salt electrolysis process of the yttrium-nickel binary intermediate alloy comprises the following steps:
respectively drying yttrium fluoride and lithium fluoride, vacuum dehydrating, mixing to obtain YF 3 : adding electrolyte LiF = 4: 1 into the electrolytic cell, heating to melt, inserting nickel cathode with phi of 30mm into the electrolyte, and inserting Y into the electrolyte 2 O 3 Continuously adding into electrolyte at uniform speed, electrolyzing with DC with average current intensity of 1500A and cathode current density of 10A/cm 2 The electrolysis temperature is maintained at 1000-1030 ℃, 1850g of yttrium oxide is added per hour, about 1950g of intermediate alloy can be obtained per hour of electrolysis on average, the intermediate alloy is discharged every 4 hours, the current efficiency is 80 percent, and the yield of metal yttrium is 95 percent. The composition of the electrolytic metal product is shown in the table.
Example A product ingredient Table
| Item | Y | Ni | C | Fe |
| Index wt% | 73 | 27 | 0.015 | 0.10 |
Example 2: the molten salt electrolysis process of the yttrium-nickel binary intermediate alloy comprises the following steps:
respectively drying yttrium fluoride and lithium fluoride, vacuum dehydrating, mixing to obtain YF 3 LiF = 6: 1 electrolyte is added into the electrolytic bath, heated to melt, a nickel cathode with a cross-sectional dimension of 10mm × 20mm is inserted into the electrolyte, and Y is added 2 O 3 Continuously adding into electrolyte at constant speed, electrolyzing with DC at average current intensity of 700A and cathode current density of 15A/cm 2 The electrolysis temperature is maintained at 1020-1050 ℃, 900g of yttrium oxide is added per hour, about 800g of intermediate alloy can be obtained per hour of electrolysis on average, the intermediate alloy is discharged once every 5 hours, the current efficiency is 80%, and the yield of yttrium metal is 93%. The composition of the electrolytic metal product is shown in the table.
EXAMPLE two product ingredient Table
| Item | Y | Ni | C | Fe |
| Index wt% | 82 | 18 | 0.018 | 0.11 |
Example 3: molten salt electrolysis process of yttrium-nickel binary intermediate alloy
Respectively drying yttrium fluoride and lithium fluoride, vacuum dehydrating, mixing to obtain YF 3 LiF = 6: 1 electrolyte is added into the electrolytic bath, heated to melt, two phi 30mm nickel cathodes are inserted into the electrolyte side by side, Y is added 2 O 3 Continuously adding into electrolyte at constant speed, electrolyzing with DC at average current intensity of 1200A and cathode current density of 12A/cm 2 The electrolysis temperature is maintained at 1050-1080 ℃, 1500g of yttrium oxide is added per hour, about 1500g of intermediate alloy can be obtained per hour of electrolysis on average, the intermediate alloy is discharged every 3 hours, the current efficiency is 80%, and the yield of yttrium metal is 94%. The composition of the electrolytic metal product is shown in the table.
EXAMPLES three product ingredient lists
| Item | Y | Ni | C | Fe |
| Index wt% | 75 | 25 | 0.02 | 0.11 |
Example 4: molten salt electrolysis process of lanthanum-yttrium-nickel ternary intermediate alloy
Lanthanum fluoride, yttrium fluoride and lithium fluoride are respectively dried and dehydrated in vacuum, and then mixed to prepare LaF with weight ratio 3 ∶YF 3 Adding electrolyte of LiF = 3.5: 4: 1 into the electrolytic tank, heating to melt the electrolyte, inserting a nickel cathode with phi of 40mm into the electrolyte, and adding La in the weight ratio 2 O 3 ∶Y 2 O 3 Adding the mixture of 1: 1.5 into electrolyte at constant speed, electrolyzing with direct current with average current intensity of 3000A and cathode current density of 10A/cm 2 The electrolysis temperature is maintained at 1050-1080 ℃, 4100g of mixed oxide is added per hour, about 4500g of intermediate alloy can be obtained per hour of electrolysis on average, the intermediate alloy is discharged once every 3 hours, the current efficiency is 80%, and the rare earth yield is 94%. The composition of the electrolytic metal product is shown in the table.
EXAMPLE four product ingredient Table
| Item | La | Y | Ni | C | Fe |
| Index wt% | 30 | 43 | 27 | 0.017 | 0.11 |
Example 5: molten salt electrolysis process of yttrium-nickel binary intermediate alloy
Respectively drying yttrium fluoride, lithium fluoride and calcium fluoride, vacuum dehydrating, mixing, and preparing YF 3 ∶LiF∶CaF 2 Adding electrolyte of = 6: 1: 0.5 into electrolytic tank, heating to melt, inserting nickel cathode of phi 25mm into electrolyte, and adding Y 2 O 3 Continuously adding into electrolyte at constant speed, electrolyzing with DC at average current intensity of 1000A and cathode current density of 10A/cm 2 The electrolysis temperature is maintained at 1000-1040 ℃, 1250g of yttrium oxide per hour, about 1150g of intermediate alloy can be obtained per hour of electrolysis on average, the intermediate alloy is discharged once every 5 hours, the current efficiency is 80 percent, and the rare earth yield is 95 percent. The composition of the electrolytic metal product is shown in the table.
EXAMPLE five ingredient Table
| Item | Y | Ni | C | Fe |
| Index wt% | 80 | 20 | 0.013 | 0.1 |
Example 6: molten salt electrolysis process of lanthanum-cerium-yttrium-nickel quaternary intermediate alloy
Lanthanum fluoride, cerium fluoride, yttrium fluoride and lithium fluoride are respectively dried and dehydrated in vacuum, and then are mixed to prepare LaF with the weight ratio 3 ：CeF 3 ：YF 3 : adding electrolyte of LiF = 3: 1: 4: 1 into the electrolytic tank, heating to melt the electrolyte, inserting a nickel cathode with phi of 40mm into the electrolyte, and adding La in weight ratio 2 O 3 ：CeO 2 ：Y 2 O 3 Adding a mixture of = 2: 1: 4 into an electrolyte continuously at a constant speed, electrifying direct current for electrolysis, wherein the average current intensity is 2000A, the cathode current density is 10A/cm < 2 >, the electrolysis temperature is maintained at 1050-1080 ℃, 2800g of mixed oxide is added per hour, about 3000g of intermediate alloy can be obtained per hour of electrolysis, the intermediate alloy is discharged every 3 hours, the current efficiency is 80%, and the rare earth yield is 94%. The composition of the electrolytic metal product is shown in the table.
EXAMPLE six product ingredient Table
| Item | La | Ce | Y | Ni | C | Fe |
| Index wt% | 20 | 10 | 45 | 25 | 0.015 | 0.11 |
Example 7: molten salt electrolysis process of yttrium-nickel binary intermediate alloy
Respectively drying yttrium fluoride and lithium fluoride, vacuum dehydrating, mixing to obtain YF 3 Adding electrolyte of LiF = 4: 1 into the electrolytic bath, heating to melt the electrolyte, inserting a nickel cathode with phi of 26mm into the electrolyte, and inserting Y into the electrolyte 2 O 3 Continuously adding into electrolyte at constant speed, electrolyzing with DC at average current intensity of 300A and cathode current density of 8A/cm 2 The electrolysis temperature is maintained at 1000-1030 ℃, 350g of yttrium oxide is added per hour, about 600g of intermediate alloy can be obtained per hour of electrolysis on average, the current efficiency is 80%, and the yield of yttrium metal is 94%. The composition of the electrolytic metal product is shown in the table.
EXAMPLE seven product ingredient Table
| Item | Y | Ni | C | Fe |
| Index wt% | 50 | 50 | 0.018 | 0.10 |
Example 8: molten salt electrolysis process of yttrium-nickel binary intermediate alloy
Mixing yttrium fluoride and lithium fluoride after respective drying and vacuum dehydration steps to prepare YF in weight ratio 3 Adding electrolyte of LiF = 4: 1 into the electrolytic bath, heating to melt the electrolyte, inserting two nickel cathodes phi of 26mm into the electrolyte side by side, and inserting Y into the electrolyte 2 O 3 Continuously adding into electrolyte at constant speed, electrolyzing with DC at average current intensity of 300A and cathode current density of 10A/cm 2 The electrolysis temperature is maintained at 900-950 ℃, 350g of yttrium oxide is added per hour, about 345g of intermediate alloy can be obtained per hour of electrolysis on average, the current efficiency is 70%, and the yield of yttrium metal is 94%. The composition of the electrolytic metal product is shown in the table.
EXAMPLE eight ingredient Table
| Item | Y | Ni | C | Fe |
| Index wt% | 77 | 23 | 0.015 | 0.11 |
Claims (1)
1. A molten salt electrolysis process of a yttrium-nickel binary intermediate alloy is characterized by comprising the following steps:
respectively drying yttrium fluoride, lithium fluoride and calcium fluoride, vacuum dehydrating, mixing, and preparing YF 3 ∶LiF∶CaF 2 Adding electrolyte of = 6: 1: 0.5 into electrolytic tank, heating to melt, inserting nickel cathode of phi 25mm into electrolyte, and adding Y 2 O 3 Continuously adding into electrolyte at constant speed, electrolyzing with DC at average current intensity of 1000A and cathode current density of 10A/cm 2 Maintaining the electrolysis temperature at 1000-1040 ℃, adding 1250g of yttrium oxide per hour, taking a graphite crucible as an electrolytic bath and a graphite block as an anode, and discharging 1150g of intermediate alloy per hour of electrolysis on average, wherein the discharging is performed once every 5 hours, the current efficiency is 80%, and the rare earth yield is 95%;
the composition of the master alloy is as follows:
。
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| CN109913700B (en) * | 2019-04-30 | 2020-10-27 | 三桥惠(佛山)新材料有限公司 | Preparation method of surface micro-porous nickel-plated hydrogen storage alloy |
| CN110359064B (en) * | 2019-08-26 | 2021-03-05 | 包头市三隆稀有金属材料有限责任公司 | Preparation method of lanthanum-yttrium alloy |
| CN112921363B (en) * | 2019-12-05 | 2022-05-10 | 有研稀土新材料股份有限公司 | Preparation method of yttrium-nickel hydrogen storage alloy |
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| CN112267131B (en) * | 2020-10-23 | 2022-03-11 | 赣州有色冶金研究所有限公司 | Yttrium-nickel alloy and preparation method and application thereof |
| CN115305523B (en) * | 2021-05-08 | 2023-11-03 | 中南大学 | Preparation method of rare earth alloy |
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| CN115852163A (en) * | 2022-11-23 | 2023-03-28 | 包头稀土研究院 | Separation method of rare earth zinc alloy |
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