CN103074643B - The method of different Ni-Tb intermetallic compound is prepared in fused salt electrolysis - Google Patents
The method of different Ni-Tb intermetallic compound is prepared in fused salt electrolysis Download PDFInfo
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Abstract
The present invention is to provide a kind of method that different Ni-Tb intermetallic compound is prepared in fused salt electrolysis.LiCl:KCl:TbCl is consisted of according to mass ratio in electrolyzer
3the ratio of=43.90% ~ 44.0%:52.03% ~ 52.11%:3.97% ~ 3.99% adds ionogen, at temperature 500 ~ 800 DEG C, add a cover and be heated to complete melting, employing metallic nickel is negative electrode, graphite rod is anode, Ag/AgCl is reference electrode, and control cathode carries out electrolysis 2 ~ 8 hours relative to the current potential of Ag/AgCl reference electrode at-1.7V ~-2.2V, solid state N i electrode separates out Tb and diffuses to form containing Ni to Ni cathode internal
17tb
2, Ni
5tb and Ni
2the intermetallic compound of Tb and Ni-Tb alloy.The present invention, by control cathode current potential, forms different Ni-Tb intermetallic compound.Wherein Tb and Ni can form the Ni with higher fusing point and good high temperature corrosion
5tb and Ni
2tb strengthening phase.
Description
Technical field
That the present invention relates to is a kind of preparation method of Ni-Tb intermetallic compound.
Background technology
Nickel-based intermetallic compound and alloy thereof, due to its good oxidation-resistance and corrosion resistance nature, there is certain application in the field such as chemical industry, electronics.And rare earth element is due to its crystal grain thinning, the characteristic strengthening the corrosion-resistant and alloy creep of alloy, it is a kind of main alloy element of nickel-base alloy.In nickel-based intermetallic compound and alloy thereof, add rare earth element can improve its casting, corrosion-resistant and Creep Properties.And rare earth element tb is having beyond above advantage, Ni can formed with nickel
5tb and Ni
2tb intermetallic compound, these two kinds of intermetallic compounds have magnetocrystalline anisotropy and magnetic heating performance, add Fe and carry out composition adjustment and adulterate studying, can prepare Tb-Ni-Fe system giant magnetostrictive material.
Because Tb-Ni-Fe system giant magnetostrictive material not only has Magnetostriction significantly, and there is excellent processing characteristics, the exploitation that can be new device provides material foundation, has broad application prospects in high-power underwater communication, high-precision micro motor, hydraulic pressure and the field such as Valve controlling, precision sizing.
Traditional main method preparing nickel-based intermetallic compound production has pressure sintering and powder metallurgic method.Pressure sintering, such as publication number is CN1388265, name is called in the patent document of " hot-pressing process of polycrystalline intermetallic Ni-Al compound ", disclose a kind of method that pressure sintering prepares intermetallic Ni-Al compound, nickel aluminium sample is embedded in the coated overcoat of stainless steel, is heated to 1000-1200 DEG C, the draught of employing 5-15% and Deformation velocity are 1000-1200 DEG C of cogging, the final pressure temperature 600-1000 DEG C of deflection once suppressed to specifying, 300-800 DEG C of insulation, is then cooled to room temperature.Powder metallurgic method, such as publication number is CN102140603, and name is called " with nickel-Al intermetallic Ni
3al is Wimet and the preparation method of Binder Phase " patent document in, disclose a kind of nickel-Al intermetallic Ni
3al is the Wimet of Binder Phase and the method for preparation.A certain proportion of metallic nickel, aluminium powder form are loaded on crystal vessel middle berth mean longitude and cross heating and thermal insulation, mills, broken, sieve, obtain carbide and the Ni of less than 120 microns
3the mixture of Al, carries out deoxidation pre-treatment; Mix with the B powder wet-milling of certain mass mark, make pressed compact; Pressed compact obtains nickel-Al intermetallic after 1350 ~ 1550 DEG C of low pressure liquid phase sintering.
At present, about the report adopting fused salt electrolysis process directly to prepare nickelalloy in prior art, be such as CN101768763A at publication number, name is called in " method and apparatus that magnesium-nickel alloy is prepared in a kind of fused salt electrolysis ", disclose one to mix Sodium Fluoride and magnesium fluoride as molten salt system, add magnesium oxide, employing metal nickel plate is negative electrode, graphite rod is anode, is heated to 900 ~ 1200 DEG C and carries out constant-current electrolysis.Current density is 0.5 ~ 1A/cm
2, electrolysis time is 0.4 ~ 1.5h, and obtaining MAGNESIUM METAL mass content is the magnesium-nickel alloy of 1.5 ~ 17%.
Summary of the invention
The object of the present invention is to provide a kind of method that energy consumption is low, different Ni-Tb intermetallic compound is prepared in fused salt electrolysis that is that can prepare different Ni-Tb intermetallic compound.
The object of the present invention is achieved like this:
LiCl:KCl:TbCl is consisted of according to mass ratio in electrolyzer
3the ratio of=43.90% ~ 44.0%:52.03% ~ 52.11%:3.97% ~ 3.99% adds ionogen, at temperature 500 ~ 800 DEG C, add a cover and be heated to complete melting, metallic nickel (Ni) is adopted to be negative electrode, graphite rod is anode, Ag/AgCl is reference electrode, and control cathode carries out electrolysis 2 ~ 8 hours relative to the current potential of Ag/AgCl reference electrode at-1.7V ~-2.2V, solid state N i electrode separates out Tb and diffuses to form containing Ni to Ni cathode internal
17tb
2, Ni
5tb and Ni
2the intermetallic compound of Tb and Ni-Tb alloy.
Described NaCl, KCl are respectively 300 DEG C, 600 DEG C dryings 24 hours.
Feature of the present invention is mainly reflected in:
(1) the present invention is to provide a kind of by regulating temperature and electropotential prepare different Ni-Tb intermetallic compound and control the method for phase composite.Following table is for prepare different Ni-Tb intermetallic compound by the inventive method.Electrolyte temperature 500 ~ 800 DEG C, control cathode current potential at-1.7 ~-2.2V(relative to Ag/AgCl reference electrode), electrolysis time 2 ~ 8 hours.Result is as follows:
Wherein Ni
2tb and Ni
5tb is strengthening phase, has higher fusing point, high-temperature corrosion resistance.The present invention can prepare the Ni-Tb intermetallic compound of strengthening phase by control electrolysis temperature and electropotential.
(2) overall electrolysis process mainly contains controlled-potential electrolysis and controls current electroanalysis.Controlled-potential electrolysis is the most effective means realizing overall electrolysis, can obtain pre-prepared intermetallic compound by permanent potential electrolysis.
(3) electrolysis temperature of the present invention low (740 ~ 780 DEG C), well below W metal (1453 DEG C), Tb(1360 DEG C) fusing point, therefore, can work-ing life of extension device, save energy, reduces production cost.
Accompanying drawing explanation
Accompanying drawing 1 is that the XRD figure containing different Ni-Tb intermetallic compound prepared by embodiment 1,2 and 3 is composed.As can be seen from the figure, Tb is with Ni
17tb
2, Ni
5tb and Ni
2the form of the intermetallic compound of Tb phase is present in alloy phase.Ni
5tb and Ni
2tb is strengthening phase, has higher fusing point, high-temperature corrosion resistance.
Embodiment
Illustrate below and the present invention is described in more detail.
Embodiment 1: in electrolyzer, in system, each electrolytical quality proportioning is LiCl:KCl:TbCl
3=43.90%:52.11%:3.99%.Add a cover after being heated to 500 DEG C of complete meltings, metallic nickel (Ni) is adopted to be negative electrode, graphite rod is anode, Ag/AgCl is reference electrode, at temperature 500 DEG C, at-2.2V(relative to Ag/AgCl reference electrode) carry out potentiostatic deposition 2 hours, solid state N i electrode separates out Tb and diffuses to form containing Ni to Ni cathode internal
17tb
2and Ni
2the intermetallic compound of Tb.
Embodiment 2: in electrolyzer, in system, each electrolytical quality proportioning is LiCl:KCl:TbCl
3=44.00%:52.03%:3.97%.Add a cover after being heated to 700 DEG C of complete meltings, metallic nickel (Ni) is adopted to be negative electrode, graphite rod is anode, Ag/AgCl is reference electrode, at temperature 700 DEG C, at-2.2V(relative to Ag/AgCl reference electrode) carry out potentiostatic deposition 5 hours, solid state N i electrode separates out Tb and diffuses to form containing Ni to Ni cathode internal
2the intermetallic compound of Tb.
Embodiment 3: in electrolyzer, in system, each electrolytical quality proportioning is LiCl:KCl:TbCl
3=43.95%:52.06%:3.99%.Add a cover after being heated to 800 DEG C of complete meltings, metallic nickel (Ni) is adopted to be negative electrode, graphite rod is anode, Ag/AgCl is reference electrode, at temperature 800 DEG C, at-1.7V(relative to Ag/AgCl reference electrode) carry out potentiostatic deposition 8 hours, solid state N i electrode separates out Tb and diffuses to form containing Ni to Ni cathode internal
5the intermetallic compound of Tb.
Claims (2)
1. a method for different Ni-Tb intermetallic compound is prepared in fused salt electrolysis, it is characterized in that: consist of LiCl:KCl:TbCl according to mass ratio in electrolyzer
3the ratio of=43.90% ~ 44.0%:52.03% ~ 52.11%:3.97% ~ 3.99% adds ionogen, at temperature 500 ~ 800 DEG C, add a cover and be heated to complete melting, employing metallic nickel is negative electrode, graphite rod is anode, Ag/AgCl is reference electrode, control cathode carries out electrolysis 2 ~ 8 hours relative to the current potential of Ag/AgCl reference electrode at-1.7V ~-2.2V, solid state N i electrode separate out Tb and diffuse to form intermetallic compound to Ni cathode internal, being specially the one in following intermetallic compound:
(1) electrolysis temperature is 500 DEG C, and control cathode is-2.2V relative to the current potential of Ag/AgCl reference electrode, carries out potentiostatic deposition and obtains containing Ni for 2 hours
17tb
2and Ni
2the intermetallic compound of Tb;
(2) electrolysis temperature is 700 DEG C, and control cathode is-2.2V relative to the current potential of Ag/AgCl reference electrode, carries out potentiostatic deposition 5 hours, obtains containing Ni
2the intermetallic compound of Tb;
(3) electrolysis temperature is 800 DEG C, and control cathode is-1.7V relative to the current potential of Ag/AgCl reference electrode, carries out potentiostatic deposition and obtains containing Ni for 8 hours
5the intermetallic compound of Tb.
2. the method for different Ni-Tb intermetallic compound is prepared in fused salt electrolysis according to claim 1, it is characterized in that: described LiCl, KCl are respectively 300 DEG C, 600 DEG C dryings 24 hours.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101109090A (en) * | 2007-07-24 | 2008-01-23 | 哈尔滨工程大学 | Method for producing out-phase compositive magnesium lithium alloy with low-temperature electrolyzing |
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| JP2964649B2 (en) * | 1991-01-17 | 1999-10-18 | 三菱化学株式会社 | Method for producing terbium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101109090A (en) * | 2007-07-24 | 2008-01-23 | 哈尔滨工程大学 | Method for producing out-phase compositive magnesium lithium alloy with low-temperature electrolyzing |
Non-Patent Citations (1)
| Title |
|---|
| Electrochemical Formation of Tb-Ni Alloys in a Molten LiCl-KCl-TbCl3 System;H. Konishi等;《18th International Symposium on Molten Salts and Ionic Liquids as part of the 222nd Meeting of the Electrochemical-Society》;20121231;第50卷(第11期);实验部分及结果与讨论部分 * |
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