CN104480492B - A kind of method that ionic liquid electrodeposition prepares Ni La alloys - Google Patents
A kind of method that ionic liquid electrodeposition prepares Ni La alloys Download PDFInfo
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Abstract
The present invention relates to a kind of method that ionic liquid electrodeposition prepares Ni La alloys, belong to non-ferrous metallurgy technology technical field.First under controlled atmosphere, additive, nickel salt and lanthanum salt are sequentially added in ionic liquid, be well mixed to obtain il electrolyte;Used as negative electrode, graphite or other inert materials are anode to the matrix that will be pre-processed, and it is 0.2 ~ 5cm with cathode distance to keep anode, is 5 ~ 20mA/m in current density2, temperature be 60 ~ 100 DEG C at carry out galvanostatic deposition 1 ~ 6 hour, then take out negative electrode, through flushing and drying after, obtain final product Ni La alloy depositions layer.The method operation temperature is low, less energy consumption, and the corrosivity to equipment is small, environment-friendly, with low cost, the problems such as solving vapour deposition process equipment requirement high, high cost, should not largely prepare.
Description
Technical field
The present invention relates to a kind of method that ionic liquid electrodeposition prepares Ni-La alloys, belong to non-ferrous metallurgy technology
Technical field.
Background technology
Nickel lanthanum alloy has the excellent properties such as catalysis activity is high, hydrogen storage property is good and corrosion resistance is strong, is widely used in green
The numerous areas such as color Ni-MH battery, catalytic hydrogenation, anti-corrosion of metal.But nickel lanthanum alloy film is prepared at present mainly uses ion
The physical vapour deposition (PVD)s such as plating, cathodic sputtering, have that equipment is complicated, high cost, the defect such as should not produce in enormous quantities.
Electrodeposition process is simple due to operation and equipment, sedimentary can be controlled to constitute by adjusting electro-deposition process parameter,
The advantages of thickness, pattern and crystalline state, as one of effective ways for preparing alloy firm.But the reduction potential of lanthanum ion is relatively born
(-2.38Vvs.SHE), differ larger with the reduction potential of nickel ion, it is difficult to electro-deposition is out from aqueous solution electro-deposition.This
Outward, hydrogen inevitably separates out in aqueous solution electrolysis liquid during electro-deposition, the full absorption of gas will hinder metal in substrate
Deposition, cause sedimentary uneven.Although hydrogen is avoided using the organic solvent and high-temperature molten salt electro-deposition of non-aqueous system
Precipitation, but organic solvent high volatility, electrochemical window relative narrower, the solvability to lanthanum salt are low, it is difficult to obtain content of magnesium
Alloy film high, and field trash is more, it is coarse not fine and close;High-temperature molten salt is serious to equipment corrosion, depositing temperature is higher, energy consumption
Larger, coating easily produces dendrite or efflorescence, second-rate.Therefore, to obtain preparing Ni-La alloy layers, in the urgent need to one
The more preferable solvent of performance is planted as electrolyte, the nothing that occurs of ionic liquid provides new possibility suspected of this.
Ionic liquid is that one kind is made up of anions and canons, in the organic salt that room temperature or near room temperature are in a liquid state, with electrification
Learn that window is wide, good conductivity, liquid state range are wide, without excellent properties such as vapour pressure, good stabilities, be a kind of green solvent.In electricity
Deposition aspect, ionic liquid has merged the advantage of high-temperature molten salt and the aqueous solution:With electrochemical window wider and good lead
Electrically, the metal and alloy that ability electro-deposition goes out in high-temperature molten salt are can obtain at room temperature, but it is such without high-temperature molten salt
Severe corrosive;Meanwhile, electrodepositable is gone back in ionic liquid and obtains most of metals that can be obtained in aqueous, and without pair
Reaction, more preferably, current efficiency is higher for metal quality because obtained from, electricity in aqueous is particularly difficult to aluminium, magnesium, titanium etc. heavy
The metal and its alloy that product is obtained are even more so.The above-mentioned characteristic and its good electrical conductivity of ionic liquid make electro-deposition
The brand-new liquid of research, is more and more applied in terms of electrodeposit metals.
The content of the invention
For problem and deficiency that above-mentioned prior art is present, the present invention provides a kind of ionic liquid electrodeposition and prepares Ni-
The method of La alloys.The method operation temperature is low, less energy consumption, and the corrosivity to equipment is small, environment-friendly, with low cost, solves
Vapour deposition process equipment requirement is high, high cost, the problems such as should not largely prepare, the present invention is achieved through the following technical solutions.
A kind of method that ionic liquid electrodeposition prepares Ni-La alloys, its specific steps include as follows:
(1)First under controlled atmosphere, additive, nickel salt and lanthanum salt are sequentially added in ionic liquid, be well mixed
Il electrolyte is obtained, wherein additive and the mol ratio of ionic liquid is 1:0.01 ~ 2, in il electrolyte nickel from
The concentration of son is 0.02 ~ 0.2mol/L, and the concentration of lanthanum ion is 0.1 ~ 0.4mol/L;
(2)Used as negative electrode, graphite or other inert materials are anode to the matrix that will be pre-processed, and keep anode and cathode distance
It is 0.2 ~ 5cm, is 5 ~ 20mA/m in current density2, temperature be 60 ~ 100 DEG C at carry out galvanostatic deposition 1 ~ 6 hour, Ran Houqu
Go out negative electrode, through flushing and drying after, obtain final product Ni-La alloy depositions layer.
The step(1)Intermediate ion liquid is 1-ethyl-3-methyllimidazolium bromide salt(EMIB), chlorination 1- butyl -3-
Methylimidazole salt(BMIC), the methylimidazole dintrile ammonia salt of 1- butyl -3([Bmim]DCA)Or the methylimidazole of 1- butyl -3 double three
Methyl fluoride Asia amidic-salt([Bmim]TFSA).
The step(1)In additive be ethylene glycol, propane diols, glycerine, acetonitrile, butynediols or acetone.
The step(1)In nickel salt be NiCl2Or NiSO4。
The step(1)In lanthanum salt be LaCl3Or La (NO)3。
The step(2)In matrix material be copper, nickel or mild steel.
When ionic liquid is [Bmim] DCA ionic liquids, it is not necessary to any addition additive.
The beneficial effects of the invention are as follows:First, the present invention prepares Ni-La alloys using electrodeposition process, can be heavy by regulation
Product condition controls the composition of alloy, with composition is controllable, equipment and process is simple, low power consumption and other advantages, this point with it is traditional
Vapour deposition process is compared to the progress with essence;Secondly, electroreduction temperature of the present invention is low, and the present invention is using ionic liquid electrolysis
Below 100 DEG C, high-temperature molten salt electrodeposition temperature reduces 700 DEG C to reduction temperature more than 800 DEG C, largely saves
About cost, reduce energy consumption and slow down the corrosion to equipment;3rd, realize electrode potential differ larger two kinds of magnesium metals and
The co-deposition of nickel, for the alloy that two kinds of larger metals of electrode potential difference are prepared using electro-deposition provides a kind of new method;
Ionic liquid electrodeposition Ni-La alloys are finally used, Ni-La alloy of the lanthanum content control in 0.4 ~ 8.5at% is obtained, it is and existing
Ni-La alloy preparation methods compare, present invention process is simple, and low for equipment requirements, energy consumption is smaller, with low cost, obtains
Alloy layer quality is good.
Brief description of the drawings
Fig. 1 is the SEM photograph that the embodiment of the present invention 2 prepares Ni-La alloys.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The method that the ionic liquid electrodeposition prepares Ni-La alloys, its specific steps include as follows:In inert-gas environment,
By ionic liquid BMIC and ethylene glycol(EG)It is in molar ratio 1:2 ratio is well mixed, and is subsequently adding the NiCl of 0.1mol/L2
With the LaCl of 0.1mol/L3, stirring and dissolving obtains il electrolyte;By matrix copper sheet sand paper polishing grinding, use successively
0.1mol/L hydrochloric acid solutions, acetone, ethanol cleaning, as negative electrode after fully drying, graphite keeps electrolysis liquid temperature as anode
Spend for 60 DEG C, keep anode and cathode distance to be 0.2cm, control electric current density is 10mA/m2Electro-deposition 6 hours, obtains negative electrode examination
Part;Acetonitrile and distilled water flushing being used successively after taking out negative electrode test specimen, being dried, obtain final product Ni-La alloy layers, the content of lanthanum is
0.41wt%。
Embodiment 2
The method that the ionic liquid electrodeposition prepares Ni-La alloys, its specific steps include as follows:In inert-gas environment,
By ionic liquid BMIC and propane diols(GL)It is in molar ratio 1:2 ratio is well mixed, and is subsequently adding the NiCl of 0.1mol/L2
With the LaCl of 0.2mol/L3, stirring and dissolving obtains il electrolyte;By matrix copper sheet sand paper polishing grinding, use successively
0.1mol/L hydrochloric acid solutions, acetone, ethanol cleaning, as negative electrode after fully drying, graphite keeps electrolysis liquid temperature as anode
Spend for 80 DEG C, keep anode and cathode distance to be 5cm, control electric current density is 10mA/m2Electro-deposition 3 hours, obtains negative electrode test specimen;
Acetonitrile and distilled water flushing being used successively after taking out negative electrode test specimen, being dried, obtain final product Ni-La alloy layers, the content of lanthanum is
1.41wt%, the SEM photograph of the Ni-La alloys for preparing is as shown in Figure 1.
Embodiment 3
The method that the ionic liquid electrodeposition prepares Ni-La alloys, its specific steps include as follows:In inert-gas environment,
It is in molar ratio 1 by ionic liquid [Bmim] TFSA and acetone:0.01 ratio is well mixed, and is subsequently adding 0.02mol/L's
Ni(SO4)2With the La (NO) of 0.1mol/L3, stirring and dissolving obtains il electrolyte;By matrix copper sheet sand paper polishing grinding,
Cleaned with 0.1mol/L hydrochloric acid solutions, acetone, ethanol successively, as negative electrode after fully drying, graphite keeps electricity as anode
Solution liquid temperature degree is 100 DEG C, keep anode and cathode distance to be 1cm, control electric current density is 20mA/m2Electro-deposition 1 hour, obtains cloudy
Pole test specimen;Acetonitrile and distilled water flushing are used successively after taking out negative electrode test specimen, is dried, obtain final product Ni-La alloy layers, the content of lanthanum
It is 5.32wt%.
Embodiment 4
The method that the ionic liquid electrodeposition prepares Ni-La alloys, its specific steps include as follows:In inert-gas environment,
It is in molar ratio 1 by ionic liquid [Bmim] TFSA and acetonitrile:0.05 ratio is well mixed, and is subsequently adding 0.02mol/L's
NiCl2With the LaCl of 0.2mol/L3, stirring and dissolving obtains il electrolyte;By matrix mild steel sand paper polishing grinding, according to
Secondary to be cleaned with 0.1mol/L hydrochloric acid solutions, acetone, ethanol, as negative electrode after fully drying, graphite keeps electrolysis as anode
Liquid temperature degree is 80 DEG C, keep anode and cathode distance to be 3cm, control electric current density is 5mA/m2Electro-deposition 1 hour, obtains negative electrode examination
Part;Acetonitrile and distilled water flushing being used successively after taking out negative electrode test specimen, being dried, obtain final product Ni-La alloy layers, the content of lanthanum is
8.46wt%。
Embodiment 5
The method that the ionic liquid electrodeposition prepares Ni-La alloys, its specific steps include as follows:In inert-gas environment,
By the NiCl of 0.2mol/L2With the LaCl of 0.2mol/L3[Bmim] DCA ionic liquids are added to, stirring and dissolving obtains ionic liquid electricity
Solution liquid;By nickel sheet sand paper polishing grinding, cleaned with 0.1mol/L hydrochloric acid solutions, acetone, ethanol successively, made after fully drying
It is negative electrode, used as anode, it is 2cm, control electric current density for 70 DEG C, holding anode and cathode distance to keep electrolyte temperature to graphite
It is 15mA/m2Electro-deposition 4 hours, obtains negative electrode test specimen;Acetonitrile and distilled water flushing are used successively after taking out negative electrode test specimen, are dried,
Ni-La alloy layers are obtained final product, the content of lanthanum is 3.18wt%.
Embodiment 6
The method that the ionic liquid electrodeposition prepares Ni-La alloys, its specific steps include as follows:In inert-gas environment,
It is in molar ratio 1 by ionic liquid [Bmim] DCA and butynediols:0.01 ratio is well mixed, and is subsequently adding 0.1mol/L
NiCl2With the LaCl of 0.3mol/L3, stirring and dissolving obtains il electrolyte;By nickel sheet sand paper polishing grinding, use successively
0.1mol/L hydrochloric acid solutions, acetone, ethanol cleaning, as negative electrode after fully drying, graphite keeps electrolysis liquid temperature as anode
Spend for 90 DEG C, keep anode and cathode distance to be 4cm, control electric current density is 20mA/m2Electro-deposition 4 hours, obtains negative electrode test specimen;
Acetonitrile and distilled water flushing being used successively after taking out negative electrode test specimen, being dried, obtain final product Ni-La alloy layers, the content of lanthanum is
6.43wt%。
Specific embodiment of the invention is explained in detail above in conjunction with accompanying drawing, but the present invention be not limited to it is above-mentioned
Implementation method, in the ken that those of ordinary skill in the art possess, can also be before present inventive concept not be departed from
Put that various changes can be made.
Claims (5)
1. a kind of method that ionic liquid electrodeposition prepares Ni-La alloys, it is characterised in that specific steps include as follows:
(1)First under controlled atmosphere, additive, nickel salt and lanthanum salt are sequentially added in ionic liquid, be well mixed from
Sub- liquid electrolyte, wherein additive are 1 with the mol ratio of ionic liquid:0.01 ~ 2, nickel ion in il electrolyte
Concentration is 0.02 ~ 0.2mol/L, and the concentration of lanthanum ion is 0.1 ~ 0.4mol/L;
(2)Used as negative electrode, graphite or other inert materials are anode to the matrix that will be pre-processed, and holding anode is with cathode distance
0.2 ~ 5cm, is 5 ~ 20mA/m in current density2, temperature be 60 ~ 100 DEG C at carry out galvanostatic deposition 1 ~ 6 hour, then take out
Negative electrode, through flushing and drying after, obtain final product Ni-La alloy depositions layer;
Additive is ethylene glycol, propane diols, glycerine, acetonitrile, butynediols or acetone.
2. the method that ionic liquid electrodeposition according to claim 1 prepares Ni-La alloys, it is characterised in that:The step
Suddenly(1)Intermediate ion liquid is 1-ethyl-3-methyllimidazolium bromide salt, chlorination 1- butyl -3- methylimidazole salts, 1- butyl -3
Methylimidazole dintrile ammonia salt or the methylimidazole bis trifluoromethyl of 1- butyl -3 Asia amidic-salt.
3. the method that ionic liquid electrodeposition according to claim 1 prepares Ni-La alloys, it is characterised in that:The step
Suddenly(1)In nickel salt be NiCl2Or NiSO4。
4. the method that ionic liquid electrodeposition according to claim 1 prepares Ni-La alloys, it is characterised in that:The step
Suddenly(1)In lanthanum salt be LaCl3Or La (NO)3。
5. the method that ionic liquid electrodeposition according to claim 1 prepares Ni-La alloys, it is characterised in that:The step
Suddenly(2)In matrix material be copper, nickel or mild steel.
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CN105112962B (en) * | 2015-09-29 | 2017-10-03 | 哈尔滨工业大学 | The method that ionic liquid electrodeposition prepares nickel gallium alloy |
CN105543911A (en) * | 2015-12-29 | 2016-05-04 | 沈阳师范大学 | Chloride 1-heptyl-3-methylimidazole/nickel chloride system electroplating solution |
CN106757215A (en) * | 2016-12-14 | 2017-05-31 | 昆明理工大学 | A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanum nickel alloy film |
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