CN107034488A - The preparation method of magnesium cerium alloy - Google Patents
The preparation method of magnesium cerium alloy Download PDFInfo
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- CN107034488A CN107034488A CN201710203246.2A CN201710203246A CN107034488A CN 107034488 A CN107034488 A CN 107034488A CN 201710203246 A CN201710203246 A CN 201710203246A CN 107034488 A CN107034488 A CN 107034488A
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- RRTQFNGJENAXJJ-UHFFFAOYSA-N cerium magnesium Chemical compound [Mg].[Ce] RRTQFNGJENAXJJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910000636 Ce alloy Inorganic materials 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 121
- 150000000703 Cerium Chemical class 0.000 claims abstract description 59
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 52
- 230000005611 electricity Effects 0.000 claims abstract description 42
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000009792 diffusion process Methods 0.000 claims abstract description 37
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000011777 magnesium Substances 0.000 claims abstract description 12
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims description 36
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 239000003792 electrolyte Substances 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 12
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical group Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 16
- 238000005275 alloying Methods 0.000 abstract description 13
- 229910052751 metal Inorganic materials 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 9
- 239000004615 ingredient Substances 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 description 29
- 229910045601 alloy Inorganic materials 0.000 description 28
- -1 cerium salt Cerium ion Chemical class 0.000 description 12
- 230000008569 process Effects 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 229910000861 Mg alloy Inorganic materials 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000010310 metallurgical process Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000009790 rate-determining step (RDS) Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention provides a kind of preparation method of magnesium cerium alloy.This method comprises the following steps：By the mass ratio of magnesium and cerium in the magnesium cerium alloy to be prepared, prepare magnesium metal and cerium salt respectively；Using magnesium metal as liquid cathode, magnesium cerium alloy is prepared using molten-salt electrolysis diffusion method；Wherein, it is 1 that the required faraday's electricity of cerium ion electric discharge in cerium salt and the ratio being electrolysed between the electrolysis electricity of cerium salt are controlled in electrolysis diffusion process:1~1.4.Utilize above-mentioned preparation method, pass through molten-salt electrolysis diffusion method, using magnesium metal as liquid cathode, control to match uniformity between the required faraday's electricity of the cerium ion electric discharge in cerium salt and the electrolysis electricity of electrolysis cerium salt during electrolysis, the electricity ratio of the two is controlled 1:1~1.4, the content of two kinds of metal ingredients in magnesium cerium alloy product can be made substantially consistent with target content, so as to reach the purpose of effectively control alloying component.And by above-mentioned molten-salt electrolysis diffusion method, the present invention has prepared magnesium cerium alloy.
Description
Technical field
The present invention relates to alloy material preparing technical field, in particular to a kind of preparation method of magnesium cerium alloy.
Background technology
Magnesium alloy has numerous excellent property such as density low, and mechanical performance and chemical property are excellent and can reclaim
The characteristic such as utilize, thus be known as " green alloy ".Magnesium alloy is widely used in various fields such as auto industry, electronics
Product, aviation, military affairs, and its consumption has the trend increased considerably.One kind that magnesium-based cerium alloy belongs in magnesium alloy series,
It has important application in terms of the making of hydrometallurgy chloride plate.
The method of this kind of alloy of traditional mode of production is smelting process, that is, is co-doped with method：Various alloying component elements pass through each independent
Metallurgical process be made after, by its melting obtain alloy.This method flow is long, and all metallic elements therein have to pass through respectively
From metallurgical process and its then refining obtain, this process is numerous and diverse, and cost is high；Because its bulk composition is active metal,
Melting production alloy process must have inert atmosphere or vacuum environment, and metal loss rate is high, and cause the pollution of environment.
For a long time, people continuously attempt to produce alloy using fused salt electrolysis process.Wherein electrolysis diffusion method is molten-salt electrolysis
Method prepares most important one kind in alloy.It is electrolysed in diffusion method, most representative work is that the magnesium that Ram Sharma are proposed is closed
Gold electrolysis diffusion method, addition liquid aluminium, as negative electrode, electrolytic oxidation magnesium or magnesium chloride, makes magnesium be sunk on aluminium in advance in the electrolytic solution
Product obtains magnesium alloy.
However, there is no electrolysis diffusion method to prepare magnesium cerium alloy at present and effectively control the report of alloying component.
The content of the invention
It is a primary object of the present invention to provide a kind of preparation method of magnesium cerium alloy, expanded with solving electrolysis in the prior art
Arching pushing can not prepare magnesium cerium alloy, and the problem of can not effectively control magnesium cerium alloy composition.
To achieve these goals, according to an aspect of the invention, there is provided a kind of preparation method of magnesium cerium alloy, its
Comprise the following steps：By the mass ratio of magnesium and cerium in the magnesium cerium alloy to be prepared, prepare magnesium metal and cerium salt respectively；With metal
Magnesium prepares magnesium cerium alloy as liquid cathode using molten-salt electrolysis diffusion method；Wherein, in electrolysis diffusion process in control cerium salt
Cerium ion electric discharge needed for faraday's electricity and be electrolysed cerium salt electrolysis electricity between ratio be 1:1~1.4.
Further, control cerium salt in cerium ion electric discharge needed for faraday's electricity with electrolysis cerium salt electrolysis electricity it
Between ratio be 1:In 1~1.4 the step of, determined to be electrolysed the Faradaic current and electrolysis time of mixed material according to formula I, and then
Magnesium cerium alloy is obtained, wherein, formula I is：
(3m(Ce)salt/M(Ce)salt)F≤It≤1.4(3m(Ce)salt/M(Ce)salt)F
In formula I, m(Ce)saltFor the quality of cerium salt, M(Ce)saltFor the relative molecular mass of cerium salt, I is Faradaic current, t
For electrolysis time, F is Faraday constant.
Further, using electrolysis time t as total electrolysis time, into electrolytic furnace disposable, intermittent or continuity plus
Enter cerium salt, to prepare magnesium cerium alloy.
Further, cerium salt is cerium chloride.
Further, in electrolysis diffusion process, the electrolyte of use includes alkali molten salt.
Further, the composition of alkali molten salt includes the one or more in lithium chloride, sodium chloride and potassium chloride.
Further, by weight percentage, electrolyte includes 50~70% lithium chloride and 30~50% sodium chloride.
Further, in electrolysis diffusion process, electrolysis temperature is 400~900 DEG C.
Further, during fused salt electrolysis codeposition, cathode-current density is 0.5~1.5A/cm2。
Apply the technical scheme of the present invention there is provided a kind of preparation method of magnesium cerium alloy, it comprises the following steps：By institute
The mass ratio of magnesium and cerium in the magnesium cerium alloy to be prepared, prepares magnesium metal and cerium salt respectively；Using magnesium metal as liquid cathode, adopt
Magnesium cerium alloy is prepared with molten-salt electrolysis diffusion method；Wherein, needed for the cerium ion electric discharge in electrolysis diffusion process in control cerium salt
Faraday's electricity and be electrolysed cerium salt electrolysis electricity between ratio be 1:1~1.4.
Using above-mentioned preparation method, by molten-salt electrolysis diffusion method, using magnesium metal as liquid cathode, control during electrolysis
Uniformity is matched between faraday's electricity and the electrolysis electricity of electrolysis cerium salt that cerium ion in cerium salt discharges required, incite somebody to action the two
Electricity ratio control 1:Within 1~1.4, the content of two kinds of metal ingredients in magnesium cerium alloy product can be made to contain substantially with target
Amount is consistent, so as to reach the purpose of effectively control alloying component.And by above-mentioned molten-salt electrolysis diffusion method, the present invention is prepared
Magnesium cerium alloy.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.The present invention is described in detail below in conjunction with embodiment.
The application is described in further detail below in conjunction with specific embodiment, these embodiments are it is not intended that limit this
Apply for scope claimed.
As described by background section, electrolysis diffusion method of the prior art can not prepare magnesium cerium alloy, and nothing
The problem of method effectively controls magnesium cerium alloy composition.
In order to solve this problem, the invention provides a kind of preparation method of magnesium cerium alloy, it comprises the following steps：Press
The mass ratio of magnesium and cerium in the magnesium cerium alloy to be prepared, prepares magnesium metal and cerium salt respectively；Using magnesium metal as liquid cathode,
Magnesium cerium alloy is prepared using molten-salt electrolysis diffusion method；Wherein, the cerium ion electric discharge institute in electrolysis diffusion process in control cerium salt
Ratio between the faraday's electricity and the electrolysis electricity of electrolysis cerium salt that need is 1:1~1.4.
Using above-mentioned preparation method, by molten-salt electrolysis diffusion method, using magnesium metal as liquid cathode, control during electrolysis
Uniformity is matched between faraday's electricity and the electrolysis electricity of electrolysis cerium salt that cerium ion in cerium salt discharges required, incite somebody to action the two
Electricity ratio control 1:Within 1~1.4, the content of two kinds of metal ingredients in magnesium cerium alloy product can be made to contain substantially with target
Amount is consistent, so as to reach the purpose of effectively control alloying component.And by above-mentioned molten-salt electrolysis diffusion method, the present invention is prepared
Magnesium cerium alloy.
Specifically, compared to traditional molten-salt electrolysis diffusion process, the step of adding control composition in the present invention.It is right
For the alloy of magnesium cerium binary system is prepared, metal is prepared respectively by the mass ratio of magnesium and cerium in the magnesium cerium alloy to be prepared
Magnesium and cerium salt, then using magnesium metal as liquid cathode, cerium salt are put into molten-salt electrolysis diffusion are carried out in electrolytic furnace.If do not controlled
Faraday's electricity matches uniformity with electrolysis electricity, and metal ion is equally existed in the electrolyte used due to electrolytic process,
Electrolysis is separated out these metal ions in the lump easily in electrolytic process, so as to destroy the diploid of magnesium cerium alloy as impurity component
System.The present invention is based on this point, it is proposed that needed for the cerium ion electric discharge in molten-salt electrolysis dissipation period control cerium salt
Ratio between the electrolysis electricity of faraday's electricity and electrolysis cerium salt is 1:1~1.4, so equivalent to the electrolysis analysis for cerium ion
Go out to be provided with the supply sum of electrolysis electricity, so as to effectively prevent the foreign metal ion in electrolyte from separating out, effectively
The magnesium cerium content of alloy product is controlled, makes it substantially consistent with target content.
In the above-mentioned preparation method that the present invention is provided, electrolysis electricity can be controlled by electrolysis time and Faradaic current.
In a preferred embodiment, the electrolysis of the faraday's electricity and electrolysis cerium salt needed for the cerium ion electric discharge in control cerium salt
Ratio between electricity is 1:In 1~1.4 the step of, when determining the Faradaic current and the electrolysis that are electrolysed mixed material according to formula I
Between, and then magnesium cerium alloy is obtained, wherein, formula I is：
(3m(Ce)salt/M(Ce)salt)F≤It≤1.4(3m(Ce)salt/M(Ce)salt)F
In formula I, m(Ce)saltFor the quality of cerium salt, M(Ce)saltFor the relative molecular mass of cerium salt, I is Faradaic current, t
For electrolysis time, F is Faraday constant (96485C/mol).
In actual mechanical process, the value of Faradaic current can be preset, it is possible to which electrolysis time is obtained according to above formula,
So as to apply during actual electrolytic codeposition of nickel.On the contrary, electrolysis time can also be preset, such as require how long
Electrolysis is completed in time, it is possible to the size of Faradaic current is determined according to above formula.In addition it is also possible to default electrolysis time and electrolysis
Electric current, so as to be determined as the quality of the magnesium metal of liquid cathode and the quality of cerium salt according to above formula.
Electrolysis electricity is controlled using electrolysis time and Faradaic current, so as to control alloying component so that in the present invention
Preparation method can use various production technologies.In a preferred embodiment, using electrolysis time t as total electrolysis time,
Cerium salt is added to disposable, intermittent or continuity into electrolytic furnace, to prepare magnesium cerium alloy.
As it was noted above, the present invention controls electrolysis electricity by electrolysis time and Faradaic current, so as to reach cerium salt
Faraday's electricity needed for the electric discharge of middle cerium ion matches uniformity with being electrolysed between the electrolysis electricity of the cerium salt.Therefore, above-mentioned
, can be just complete by the cerium salt electrolytic deposition weighed in advance in electrolysis time t shown in Formulas I.When on this basis, to be electrolysed
Between t be total electrolysis time, into electrolytic furnace, disposable, intermittent or continuity ground cerium salt, can reach that continuity prepares magnesium cerium
The purpose of alloy.And the alloy taken out after electrolysis time t, its composition is basically identical with preset value.
In a preferred embodiment, above-mentioned cerium salt is cerium chloride.Compared to other cerium salt, cerium chloride has higher
Electrolysis performance.
The electrolyte used in above-mentioned molten-salt electrolysis diffusion process can be electrolyte commonly used in the art, and the purpose is to prop up
Hold the electron motion in electrolytic process.In a preferred embodiment, in molten-salt electrolysis diffusion process, the electrolyte of use
Including alkali molten salt.The activity of alkali metal is better than cerium, correspondingly, and cerium ion precipitation is later than in electrolytic process.Using alkali gold
Belong to fused salt as electrolyte, with reference to above-mentioned electrolysis electricity rate-determining steps, can further prevent metal impurities from entering in alloy, from
And it is more beneficial for the Composition Control of binary system alloy.It is highly preferred that the composition of alkali molten salt include lithium chloride, sodium chloride and
One or more in potassium chloride.It is highly preferred that by weight percentage, electrolyte include 50~70% lithium chloride and 30~
50% sodium chloride.
Other electrolysis process can be adjusted.In a preferred embodiment, in molten-salt electrolysis diffusion process, electricity
It is 400~900 DEG C to solve temperature.Cathode-current density is 0.5~1.5A/cm2.Under the process conditions, electrolysis diffusion process is more
It is stable, so as to be conducive to further improving the quality stability of magnesium cerium alloy product.
Beneficial effects of the present invention are further illustrated by the following examples.
Embodiment 1
Alloy is designed as Mg-5wt%Ce (wherein Ce content is 5wt%), and magnesium metal and chlorine are prepared respectively in this ratio
Change cerium.
Faradaic current is preset for dc source 2A；
By formula (3m(Ce)salt/M(Ce)salt) F=It, wherein m(Ce)saltFor the quality of cerium salt, M(Ce)saltFor the phase of cerium salt
To molecular mass, I is Faradaic current 2A, and F is Faraday constant 96485C/mol.
Electrolysis time t is calculated for 10h, using the magnesium metal of preparation as liquid cathode, is disposably added whole cerium chlorides
Enter into electrolytic furnace, carry out continuous molten-salt electrolysis diffusion.
Other electrolytic parameters are as follows：
Electrolytic anode is graphite；Dc source：2A；900 DEG C of electrolyte temperature；Cathode-current density 1A/cm2；Electrolyte
Composition：Lithium chloride 60wt%- sodium chloride 40wt%.Under the conditions of above-mentioned technological parameter, continuous electrolysis took out and closed after 10 hours
Gold, uses icp analysis cerium content.
Specific data are as shown in the table：
| Alloy is designed | Mg-5wt%Ce |
| Gained alloying component | Mg-4.6wt%Ce |
Embodiment 2
Alloy is designed as Mg-5wt%Ce (wherein Ce content is 5wt%), and magnesium metal and chlorine are prepared respectively in this ratio
Change cerium.
Faradaic current is preset for dc source 2A；
By (the 3m of formula 1.4(Ce)salt/M(Ce)salt) F=It, wherein m(Ce)saltFor the quality of cerium salt, M(Ce)saltFor cerium salt
Relative molecular mass, I is Faradaic current 2A, and F is Faraday constant 96485C/mol.
Electrolysis time t is calculated for 10h, using the magnesium metal of preparation as liquid cathode, is disposably added whole cerium chlorides
Enter into electrolytic furnace, carry out continuous molten-salt electrolysis diffusion.
Other electrolytic parameters are as follows：
Electrolytic anode is graphite；Dc source：2A；700 DEG C of electrolyte temperature；Cathode-current density 1.5A/cm2；Electrolysis
Matter is constituted：Lithium chloride 70wt%- sodium chloride 30wt%.Under the conditions of above-mentioned technological parameter, continuous electrolysis takes out after 10 hours
Alloy, uses icp analysis cerium content.
Specific data are as shown in the table：
| Alloy is designed | Mg-5wt%Ce |
| Gained alloying component | Mg-4.8wt%Ce |
Embodiment 3
Alloy is designed as Mg-5wt%Ce (wherein Ce content is 5wt%), and magnesium metal and chlorine are prepared respectively in this ratio
Change cerium.
Faradaic current is preset for dc source 2A；
By (the 3m of formula 1.4(Ce)salt/M(Ce)salt) F=It, wherein m(Ce)saltFor the quality of cerium salt, M(Ce)saltFor cerium salt
Relative molecular mass, I is Faradaic current 2A, and F is Faraday constant 96485C/mol.
Electrolysis time t is calculated for 10h, using the magnesium metal of preparation as liquid cathode, is disposably added whole cerium chlorides
Enter into electrolytic furnace, carry out continuous molten-salt electrolysis diffusion.
Other electrolytic parameters are as follows：
Electrolytic anode is graphite；Dc source：2A；400 DEG C of electrolyte temperature；Cathode-current density 0.5A/cm2；Electrolysis
Matter is constituted：Lithium chloride 50wt%- sodium chloride 50wt%.Under the conditions of above-mentioned technological parameter, continuous electrolysis takes out after 10 hours
Alloy, uses icp analysis cerium content.
Specific data are as shown in the table：
| Alloy is designed | Mg-5wt%Ce |
| Gained alloying component | Mg-4.6wt%Ce |
Embodiment 4
Alloy is designed as Mg-5wt%Ce (wherein Ce content is 5wt%), and magnesium metal and chlorine are prepared respectively in this ratio
Change cerium.
Faradaic current is preset for dc source 2A；
By (the 3m of formula 1.3(Ce)salt/M(Ce)salt) F=It, wherein m(Ce)saltFor the quality of cerium salt, M (Ce) salt is cerium
The relative molecular mass of salt, I is Faradaic current 2A, and F is Faraday constant 96485C/mol.
Electrolysis time t is calculated for 10h, using the magnesium metal of preparation as liquid cathode, is disposably added whole cerium chlorides
Enter into electrolytic furnace, carry out continuous molten-salt electrolysis diffusion.
Other electrolytic parameters are as follows：
Electrolytic anode is graphite；Dc source：2A；380 DEG C of electrolyte temperature；Cathode-current density 2.0A/cm2；Electrolysis
Matter is constituted：Lithium chloride 80wt%- sodium chloride 20wt%.Under the conditions of above-mentioned technological parameter, continuous electrolysis takes out after 10 hours
Alloy, uses icp analysis cerium content.
Specific data are as shown in the table：
| Alloy is designed | Mg-5wt%Ce |
| Gained alloying component | Mg-4.5wt%Ce |
Comparative example 1
Alloy is designed as Mg-5wt%Ce (wherein Ce content is 5wt%), and magnesium metal and chlorine are prepared respectively in this ratio
Change cerium.
Faradaic current is preset for dc source 2A；
By (the 3m of formula 0.9(Ce)salt/M(Ce)salt) F=It, wherein m(Ce)saltFor the quality of cerium salt, M(Ce)saltFor cerium salt
Relative molecular mass, I is Faradaic current 2A, and F is Faraday constant 96485C/mol.
Electrolysis time t is calculated for 10h, using the magnesium metal of preparation as liquid cathode, is disposably added whole cerium chlorides
Enter into electrolytic furnace, carry out continuous molten-salt electrolysis diffusion.
Other electrolytic parameters are as follows：
Electrolytic anode is graphite；Dc source：2A；700 DEG C of electrolyte temperature；Cathode-current density 2.0A/cm2；Electrolysis
Matter is constituted：Lithium chloride 50wt%- sodium chloride 50wt%.Under the conditions of above-mentioned technological parameter, continuous electrolysis takes out after 10 hours
Alloy, uses icp analysis cerium content.
Specific data are as shown in the table：
| Alloy is designed | Mg-5wt%Ce |
| Gained alloying component | Mg-4.0wt%Ce |
Comparative example 2
Alloy is designed as Mg-5wt%Ce (wherein Ce content is 5wt%), and magnesium metal and chlorine are prepared respectively in this ratio
Change cerium.
Faradaic current is preset for dc source 2A；
By (the 3m of formula 1.6(Ce)salt/M(Ce)salt) F=It, wherein m(Ce)saltFor the quality of cerium salt, M(Ce)saltFor cerium salt
Relative molecular mass, I is Faradaic current 2A, and F is Faraday constant 96485C/mol.
Electrolysis time t is calculated for 10h, using the magnesium metal of preparation as liquid cathode, is disposably added whole cerium chlorides
Enter into electrolytic furnace, carry out continuous molten-salt electrolysis diffusion.
Other electrolytic parameters are as follows：
Electrolytic anode is graphite；Dc source：2A；700 DEG C of electrolyte temperature；Cathode-current density 2.0A/cm2；Electrolysis
Matter is constituted：Lithium chloride 50wt%- sodium chloride 50wt%.Under the conditions of above-mentioned technological parameter, continuous electrolysis takes out after 10 hours
Alloy, uses icp analysis cerium content.
Specific data are as shown in the table：
| Alloy is designed | Mg-5wt%Ce |
| Gained alloying component | Mg-3.9wt%Ce-0.07wt%Na-0.04wt%Li |
As can be seen from the above description, the above embodiments of the present invention realize following technique effect：
Using above-mentioned preparation method, spread by molten-salt electrolysis, magnesium cerium alloy can be prepared.More importantly, it is of the invention
Faraday's electricity needed for electric discharge by controlling cerium ion during electrolysis matches uniformity with electrolysis electricity, by the electricity of the two
Amount is than control 1:Within 1~1.4, can make the contents of two kinds of metal ingredients in magnesium cerium alloy product substantially with target content one
Cause, so as to reach the purpose of effectively control alloying component.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (9)
1. a kind of preparation method of magnesium cerium alloy, it is characterised in that comprise the following steps：
By the mass ratio of magnesium and cerium in the magnesium cerium alloy to be prepared, prepare magnesium metal and cerium salt respectively；
Using the magnesium metal as liquid cathode, the magnesium cerium alloy is prepared using molten-salt electrolysis diffusion method；
Wherein, faraday's electricity needed for the cerium ion electric discharge in the cerium salt is controlled in electrolysis diffusion process is described with being electrolysed
Ratio between the electrolysis electricity of cerium salt is 1:1~1.4.
2. preparation method according to claim 1, it is characterised in that the cerium ion electric discharge institute in the control cerium salt
Ratio between the faraday's electricity and the electrolysis electricity of the electrolysis cerium salt that need is 1:In 1~1.4 the step of, according to formula I
It is determined that being electrolysed the Faradaic current and electrolysis time of the mixed material, and then the magnesium cerium alloy is obtained, wherein, the formula I
For：
(3m(Ce)salt/M(Ce)salt)F≤It≤1.4(3m(Ce)salt/M(Ce)salt)F
In the formula I, m(Ce)saltFor the quality of the cerium salt, M(Ce)saltFor the relative molecular mass of the cerium salt, I is described
Faradaic current, t is the electrolysis time, and F is Faraday constant.
3. preparation method according to claim 2, it is characterised in that using the electrolysis time t as total electrolysis time, to electricity
The cerium salt is added to disposable, intermittent or continuity in solution stove, to prepare the magnesium cerium alloy.
4. preparation method according to any one of claim 1 to 3, it is characterised in that the cerium salt is cerium chloride.
5. preparation method according to claim 4, it is characterised in that in the electrolysis diffusion process, the electrolyte of use
Including alkali molten salt.
6. preparation method according to claim 5, it is characterised in that the composition of the alkali molten salt include lithium chloride,
One or more in sodium chloride and potassium chloride.
7. preparation method according to claim 6, it is characterised in that by weight percentage, the electrolyte includes 50
~70% lithium chloride and 30~50% sodium chloride.
8. the preparation method according to claim 6 or 7, it is characterised in that in the electrolysis diffusion process, electrolysis temperature is
400~900 DEG C.
9. preparation method according to claim 8, it is characterised in that during the fused salt electrolysis codeposition, negative electrode electricity
Current density is 0.5~1.5A/cm2。
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| JP2008195969A (en) * | 2007-02-08 | 2008-08-28 | Toyohashi Univ Of Technology | Method for producing alloy ingot by molten salt electrolysis using ESR heating |
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