CN106757169A - A kind of hydrogen bearing alloy rare earth intermediate alloy and preparation method thereof - Google Patents
A kind of hydrogen bearing alloy rare earth intermediate alloy and preparation method thereof Download PDFInfo
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- CN106757169A CN106757169A CN201611134246.3A CN201611134246A CN106757169A CN 106757169 A CN106757169 A CN 106757169A CN 201611134246 A CN201611134246 A CN 201611134246A CN 106757169 A CN106757169 A CN 106757169A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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- 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
- C22C19/007—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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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
Abstract
The present invention relates to a kind of hydrogen bearing alloy rare earth intermediate alloy and preparation method thereof, contain rare earth element and nickel element in alloy simultaneously；The mass percent of rare earth element and nickel element is（40‑90）：（10‑60）.Its preparation method is：With graphite crucible as electrolytic cell, graphite block makees anode, nickel rod is consumable negative electrode, in the binary or multicomponent electrolyte system of rare earth fluoride and alkali metal or alkali earth metal fluoride composition, one or more of rare earth oxide is added, direct current is passed to, rare-earth cation is in the nickel cathode concurrent intercrescence aurification of electric discharge, the alloy dropping for reacting generation is gathered in electrolytic cell receiver, and taking out casting can obtain the hydrogen bearing alloy rare earth intermediate alloy.Its advantage is：When preparing containing rare earth, nickel element hydrogen bearing alloy with the expensive simple substance rare earth metal of the low-cost high-quality intermediate alloy fictitious hosts as raw material, the cost of hydrogen bearing alloy can be significantly reduced, be conducive to the market of hydrogen bearing alloy to apply.
Description
Technical field
The present invention relates to a kind of hydrogen bearing alloy rare earth intermediate alloy and preparation method thereof, particularly a kind of hydrogen bearing alloy is used
Binary and multielement rare earth intermediate alloy and preparation method thereof, belong to field of rare earth metallurgy.
Background technology
Hydrogen bearing alloy be it is a kind of can with hydrogen reaction generation metal hydride and reversible under proper condition discharge the green of hydrogen
Color functional material, its most successful application is the negative material as nickel-metal hydrides (Ni-MH) battery.Obtain at present
Commercially use hydrogen bearing alloy is mainly AB5Type lanthanon hydrogen storage alloy Mm (NiCoMnAl)5（Mm is norium）.
AB5The capacity of type hydrogen storage alloy（340 mAh/g）Already close to its theoretical value（372 mAh/g）, further improve and be quite stranded
Difficulty, therefore, hydrogen bearing alloy of the exploitation with higher capacity is a focus of current hydrogen bearing alloy research.
In order to improve AB5The combination property of the hydrogen bearing alloy such as type or La-Mg-Ni, researchers have been also carried out largely
Element substitution research work.China has abundant yttrium（Y）Resource, the performance that hydrogen bearing alloy is improved using yttrium is had
Important meaning, such as Luo Yongchun et al. have studied La3-xYxMgNi14（x=0-2）The phase structure and chemical property of hydrogen bearing alloy
（Luo Yongchun, Chen Jiangping, Zhang Faliang, Yan Ruxu, Kang Long, Chen Jianhong, Lanzhou University of Science ＆ Technology's journal, 2006,32（4）：20-24）,
Some valuable conclusions are drawn.Inventor discovery, rare earth-yttrium-nickel system hydrogen storage when research contains the store hydrogen alloy of yttrium
Alloy has preferable hydrogen storage property, and its discharge capacity can reach 380 more than mAh/g, beyond AB5The theory of type alloy is put
Capacitance, and with preferable cycle life, is also free of Volatile Elements in alloy, prepares relatively easy, is expected to as new one
The high capacity hydrogen storage alloy in generation.
Although hydrogen bearing alloy containing yttrium has preferable hydrogen storage property, its is relatively costly, and this is mainly due to current alloy
Middle essential element yttrium is prepared by metallothermic processes, and this preparation method is long due to technological process, and uses active metal calcium
Used as reducing agent, therefore production cost is high, causes yttrium expensive.
The content of the invention
Containing the relatively costly difficulty of rare earth, nickel hydrogen bearing alloy when doing raw material with rare earth metal the invention aims to overcome
Topic provides one kind and contains rare earth simultaneously（RE）Element and nickel（Ni）Element hydrogen bearing alloy rare earth intermediate alloy and preparation method thereof.
Technical scheme is as follows：
A kind of hydrogen bearing alloy rare earth intermediate alloy, it is characterized in that：Contain rare earth in alloy simultaneously（RE）Element and nickel（Ni）Unit
Element；The mass percent of rare earth element and nickel element is, RE:Ni=（40-90）：（10-60）.
The rare earth element is one or more in scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium and lutetium.
The preparation method of the hydrogen bearing alloy rare earth intermediate alloy is：With graphite crucible as electrolytic cell, graphite block makees sun
Pole, nickel rod is consumable negative electrode, in rare earth fluoride and the binary or multicomponent electrolyte of alkali metal or alkali earth metal fluoride composition
In system, one or more of rare earth oxide is added, pass to direct current, rare-earth cation is in the concurrent intercrescence gold of nickel cathode electric discharge
Change, the alloy dropping for reacting generation is gathered in electrolytic cell receiver, taking out casting can obtain the hydrogen bearing alloy rare earth
Intermediate alloy.
Described nickel cathode is pole, square rod or sheet material, and quantity is one or more.
The binary or multicomponent electrolyte of described rare earth fluoride and alkali metal or alkali earth metal fluoride composition, wherein dilute
The mass fraction of native fluoride is 60%-97%.
Electrolysis temperature is 900-1200 DEG C in the electrolytic process.
The electrolytic process Anodic current density is 0.3-3.0A/cm2, cathode-current density is 5-25A/cm2。
It is an advantage of the invention that：Hydrogen bearing alloy is prepared using rare earth intermediate alloy of the invention, can avoid preparing containing dilute
With expensive simple substance rare earth metal as raw material when soil, nickel element hydrogen bearing alloy, can significantly reduce and be stored up containing rare earth, nickel element
The cost of hydrogen alloy, is conducive to the market containing rare earth, nickel element hydrogen bearing alloy to apply.
Specific embodiment
A kind of hydrogen bearing alloy rare earth intermediate alloy, contains rare earth simultaneously in alloy（RE）Element and nickel（Ni）Element；It is dilute
The mass percent of earth elements and nickel element is, RE:Ni=（40-90）：（10-60）.
The rare earth element is：One or more in scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium and lutetium.
Alloy of the invention is prepared using electrolysis, basic step is as follows：
（1）Hydrogen bearing alloy rare earth intermediate alloy according to required preparation, it is determined that suitable electrolyte composition；
（2）Hydrogen bearing alloy rare earth intermediate alloy and electrolytic cell scale according to required preparation, it is determined that rational anode and cathode electricity
Current density；
（3）Negative electrode and anode are installed, is loaded by certain with the electrolyte for distributing, electrolyte is melted in the heating of short circuit anode and cathode；
（4）Adjustment electrolyzer temperature adds rare earth oxide to suitable temperature, starts normal electrolysis；
（5）In electrolytic process, oxide raw material is added with certain charging rate, negative electrode is lowered at interval of certain hour, kept
Electric current, voltage stabilization；
（6）After electrolysis a period of time, come out of the stove, ingot of casting obtains hydrogen bearing alloy rare earth intermediate alloy after cooling and demolding.
Particular content of the invention and embodiments thereof are further illustrated with reference to embodiment.
Embodiment 1：The molten-salt electrolysis technique of yttrium nickel binary intermediate alloy：
By yttrium fluoride and lithium fluoride by after respective drying, vacuum dehydration step, being mixed, it is configured to weight and compares YF3：
LiF=4：1 electrolyte is added in electrolytic cell, and heating melts it, by the nickel cathode insertion electrolyte of ф 30mm, by Y2O3Even
Continuous to be at the uniform velocity added in electrolyte, logical direct current is electrolysed, and average current intensity 1500A, cathode-current density is 10A/
cm2, electrolysis temperature maintains 1000-1030 DEG C, and yittrium oxide 1850g is added per hour, and averagely often electrolysis can go out centre in one hour
Alloy about 1950g, comes out of the stove once for every 4 hours, and current efficiency is 80%, and metallic yttrium yield is 95%.The composition of electrolytic metal product
It is as shown in the table.
The product composition table of embodiment one
| Project | Y | Ni | C | Fe |
| Index wt% | 73 | 27 | 0.015 | 0.10 |
Embodiment 2：The molten-salt electrolysis technique of yttrium nickel binary intermediate alloy：
By yttrium fluoride and lithium fluoride by after respective drying, vacuum dehydration step, being mixed, it is configured to weight and compares YF3：
LiF=6：1 electrolyte is added in electrolytic cell, and heating melts it, by sectional dimension for the nickel cathode of 10mm*20mm inserts electricity
Xie Zhizhong, by Y2O3Continuously and smoothly is added in electrolyte, and logical direct current is electrolysed, average current intensity 700A, cathode current
Density is 15A/cm2, electrolysis temperature maintains 1020-1050 DEG C, and yittrium oxide 900g is added per hour, is averagely often electrolysed one hour
Intermediate alloy about 800g can be gone out, come out of the stove once within every 5 hours, current efficiency is 80%, metallic yttrium yield is 93%.Electrolytic metal product
Composition it is as shown in the table.
The product composition table of embodiment two
| Project | Y | Ni | C | Fe |
| Index wt% | 82 | 18 | 0.018 | 0.11 |
Apply example 3：The molten-salt electrolysis technique of yttrium nickel binary intermediate alloy
By yttrium fluoride and lithium fluoride by after respective drying, vacuum dehydration step, being mixed, it is configured to weight and compares YF3：
LiF=6：1 electrolyte is added in electrolytic cell, and heating melts it, and the nickel cathode of two ф 30mm is inserted into electrolyte side by side
In, by Y2O3Continuously and smoothly is added in electrolyte, and logical direct current is electrolysed, and average current intensity 1200A, cathode current is close
It is 12A/cm to spend2, electrolysis temperature maintains 1050-1080 DEG C, and yittrium oxide 1500g is added per hour, is averagely often electrolysed one hour
Intermediate alloy about 1500g can be gone out, come out of the stove once within every 3 hours, current efficiency is 80%, metallic yttrium yield is 94%.Electrolytic metal is produced
It is as shown in the table for the composition of product.
The product component list of embodiment three
| Project | Y | Ni | C | Fe |
| Index wt% | 75 | 25 | 0.02 | 0.11 |
Embodiment 4：The molten-salt electrolysis technique of lanthanum yttrium nickel ternary intermediate alloy
By lanthanum fluoride, yttrium fluoride and lithium fluoride by after respective drying, vacuum dehydration step, being mixed, weight is configured to
Amount compares LaF3：YF3：LiF=3.5：4：1 electrolyte is added in electrolytic cell, and heating melts it, and the nickel cathode of ф 40mm is inserted
It is La by weight ratio in electrolyte2O3：Y2O3=1：1.5 mixture continuously and smoothly is added in electrolyte, and logical direct current is carried out
Electrolysis, average current intensity 3000A, cathode-current density is 10A/cm2, electrolysis temperature maintains 1050-1080 DEG C, per hour
Mixed oxide 4100g is added, averagely often electrolysis can go out intermediate alloy about 4500g for one hour, come out of the stove once within every 3 hours, electric current
Efficiency is 80%, and rare-earth yield is 94%.It is as shown in the table for the composition of electrolytic metal product.
Example IV product composition table
| Project | La | Y | Ni | C | Fe |
| Index wt% | 30 | 43 | 27 | 0.017 | 0.11 |
Embodiment 5：The molten-salt electrolysis technique of yttrium nickel binary intermediate alloy
By yttrium fluoride, lithium fluoride and calcirm-fluoride by after respective drying, vacuum dehydration step, being mixed, weight is configured to
Amount compares YF3：LiF：CaF2=6：1：0.5 electrolyte is added in electrolytic cell, and heating melts it, and the nickel cathode of ф 25mm is inserted
In electrolyte, by Y2O3Continuously and smoothly is added in electrolyte, and logical direct current is electrolysed, average current intensity 1000A, negative electrode
Current density is 10A/cm2, electrolysis temperature maintains 1000-1040 DEG C, per hour yittrium oxide 1250g, and averagely often electrolysis one is small
When can go out intermediate alloy about 1150g, come out of the stove once within every 5 hours, current efficiency is 80%, and rare-earth yield is 95%.Electrolytic metal is produced
It is as shown in the table for the composition of product.
The product composition table of embodiment five
| Project | Y | Ni | C | Fe |
| Index wt% | 80 | 20 | 0.013 | 0.1 |
Embodiment 6：The molten-salt electrolysis technique of lanthanum cerium yttrium nickel quaternary intermediate alloy
By lanthanum fluoride, cerium fluoride, yttrium fluoride and lithium fluoride by after respective drying, vacuum dehydration step, being mixed, match somebody with somebody
It is made weight and compares LaF3：CeF3：YF3：LiF=3：1：4：1 electrolyte is added in electrolytic cell, and heating melts it, by ф 40mm
Nickel cathode insertion electrolyte in, by weight ratio be La2O3：CeO2：Y2O3=2：1：4 mixture continuously and smoothly is added to electrolysis
In matter, logical direct current is electrolysed, and average current intensity 2000A, cathode-current density is 10A/cm2, electrolysis temperature maintains
, mixed oxide 2800g is added per hour, averagely often electrolysis can go out intermediate alloy about 3000g, every 3 for one hour by 1050-1080 DEG C
Hour comes out of the stove once, and current efficiency is 80%, and rare-earth yield is 94%.It is as shown in the table for the composition of electrolytic metal product.
The product composition table of embodiment six
| Project | La | Ce | Y | Ni | C | Fe |
| Index wt% | 20 | 10 | 45 | 25 | 0.015 | 0.11 |
Apply example 7：The molten-salt electrolysis technique of yttrium nickel binary intermediate alloy
By yttrium fluoride and lithium fluoride by after respective drying, vacuum dehydration step, being mixed, it is configured to weight and compares YF3：
LiF=4：1 electrolyte is added in electrolytic cell, and heating melts it, by the nickel cathode insertion electrolyte of root ф 26mm, by Y2O3
Continuously and smoothly is added in electrolyte, and logical direct current is electrolysed, and average current intensity 300A, cathode-current density is 8A/
cm2, electrolysis temperature maintains 1000-1030 DEG C, and yittrium oxide 350g is added per hour, and averagely often electrolysis can go out middle conjunction in one hour
Gold about 600g, current efficiency is 80%, and metallic yttrium yield is 94%.It is as shown in the table for the composition of electrolytic metal product.
The product composition table of embodiment seven
| Project | Y | Ni | C | Fe |
| Index wt% | 50 | 50 | 0.018 | 0.10 |
Apply example 8：The molten-salt electrolysis technique of yttrium nickel binary intermediate alloy
By yttrium fluoride and lithium fluoride by after respective drying, vacuum dehydration step, being mixed, it is configured to weight and compares YF3：
LiF=4：1 electrolyte is added in electrolytic cell, and heating melts it, and the nickel cathode of two ф 26mm is inserted into electrolyte side by side
In, by Y2O3Continuously and smoothly is added in electrolyte, and logical direct current is electrolysed, average current intensity 300A, cathode-current density
It is 10A/cm2, electrolysis temperature maintains 900-950 DEG C, yittrium oxide 350g is added per hour, during averagely often electrolysis can go out for one hour
Between alloy about 345g, current efficiency is 70%, metallic yttrium yield be 94%.It is as shown in the table for the composition of electrolytic metal product.
The product composition table of embodiment eight
| Project | Y | Ni | C | Fe |
| Index wt% | 77 | 23 | 0.015 | 0.11 |
Claims (7)
1. a kind of hydrogen bearing alloy rare earth intermediate alloy, it is characterized in that：Contain rare earth in alloy simultaneously（RE）Element and nickel（Ni）
Element；The mass percent of rare earth element and nickel element is, RE:Ni=（40-90）：（10-60）.
2. hydrogen bearing alloy rare earth intermediate alloy according to claim 1, it is characterized in that：The rare earth element be scandium, yttrium,
One or more in lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium and lutetium.
3. a kind of preparation method for preparing the hydrogen bearing alloy rare earth intermediate alloy described in any one of claim 1 or 2, its feature
It is：With graphite crucible as electrolytic cell, graphite block makees anode, and nickel rod is consumable negative electrode, in rare earth fluoride and alkali metal or alkaline earth
In the binary or multicomponent electrolyte system of metal fluoride composition, one or more of rare earth oxide is added, passes to direct current,
Rare-earth cation is gathered in electrolytic cell receiver, takes in the nickel cathode concurrent intercrescence aurification of electric discharge, the alloy dropping for reacting generation
The hydrogen bearing alloy rare earth intermediate alloy is obtained by going out casting.
4. the preparation method of hydrogen bearing alloy rare earth intermediate alloy according to claim 3, it is characterized in that：Described nickel is cloudy
Extremely can be pole, square rod or sheet material, quantity is one or more.
5. the preparation method of hydrogen bearing alloy rare earth intermediate alloy according to claim 3, it is characterized in that：Described rare earth
The binary or multicomponent electrolyte of fluoride and alkali metal or alkali earth metal fluoride composition, the wherein mass fraction of rare earth fluoride
It is 60%-97%.
6. the preparation method of hydrogen bearing alloy rare earth intermediate alloy according to claim 3, it is characterized in that：It is described to be electrolysed
Electrolysis temperature is 900-1200 DEG C in journey.
7. the preparation method of hydrogen bearing alloy rare earth intermediate alloy according to claim 3, it is characterized in that：It is described to be electrolysed
Journey Anodic current density is 0.3-3.0A/cm2, cathode-current density is 5-25A/cm2。
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| CN109913700A (en) * | 2019-04-30 | 2019-06-21 | 三桥惠(佛山)新材料有限公司 | A kind of preparation method of surface micropore nickel plating hydrogen bearing alloy |
| CN110359064A (en) * | 2019-08-26 | 2019-10-22 | 包头市三隆稀有金属材料有限责任公司 | The preparation method of lanthanum yittrium alloy |
| CN112159993A (en) * | 2020-09-24 | 2021-01-01 | 赣州有色冶金研究所 | Yttrium-containing mixed rare earth metal, rare earth hydrogen storage alloy and preparation method thereof |
| CN112267131A (en) * | 2020-10-23 | 2021-01-26 | 赣州有色冶金研究所 | Yttrium-nickel alloy and preparation method and application thereof |
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| CN113517138A (en) * | 2021-06-29 | 2021-10-19 | 西安交通大学 | Method for reducing working internal pressure of aluminum electrolytic capacitor by using hydrogen storage alloy |
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