CN108728876A - A kind of preparation method of FeCoNiCuMo high-entropy alloys film - Google Patents
A kind of preparation method of FeCoNiCuMo high-entropy alloys film Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of FeCoNiCuMo high-entropy alloys film, are made into electroplate liquid by solvent of deionized water, are made up of electrochemical deposition method；Step is：S1, three parts of deionized waters are taken, triethanolamine, Ammonium Molybdate Tetrahydrate and mantoquita is dissolved in first part of deionized water, solution A is obtained；S2, glycine, ethylene glycol, antioxidant, additional salt are dissolved in second part of deionized water, obtain solution B；S3, trisodium citrate, divalent iron salt, cobalt salt, nickel salt are dissolved in third part deionized water, obtain solution C；S4, solution A, solution B and solution C are uniformly mixed, are aged, adjusted solution ph 7-8, be heated to 30 DEG C, led to nitrogen deoxygenation, obtain electroplate liquid；As anode, copper-based conduct cathode is electroplated, and FeCoNiCuMo high-entropy alloy films are obtained for S5, graphite cake.This method has the characteristics that equipment, simple for process, production efficiency is high, production cost is low, safety reliability is high, is suitable for the industrialized production of high-entropy alloy film.
Description
Technical field
The present invention relates to novel alloy thin-film material technical fields, and in particular to a kind of FeCoNiCuMo high-entropy alloys film
Preparation method.
Background technology
High-entropy alloy is the element constituent element by five or more according to equal atomic ratios or the nearly solid solution for waiting atomic ratio alloys
Phase alloy.The excellent properties that high-entropy alloy has some conventional alloys materials incomparable, such as high intensity, high rigidity, height are resistance to
Mill property, high-corrosion resistance, high thermal resistance, high resistance etc. make it have very high application value and foreground in materialogy field, with
Most there are three big hot spots of development potentiality in large block amorphous, composite material and referred to as coming few decades.High-entropy alloy is attached to matrix
Surface can also show the performance as high-entropy alloy when forming film, high-entropy alloy can be reduced by preparing high-entropy alloy film
Manufacturing cost becomes the widely applied breach of high-entropy alloy.The preparation method of high-entropy alloy mainly have melting, sintering,
Electrolysis, such as vacuum non-consumable electrode arc melting, the melting of inert gas atmosphere negative-pressure vacuum, electromagnetic levitation-melt, electric discharge etc.
Ion sintering, Self- propagating Sintering Synthetic, oxide and salt melt electrolyzing etc..The preparation method of high-entropy alloy film is mainly magnetron sputtering
Method.Electro-deposition rule is to prepare method most simple and fast in a variety of methods of high-entropy alloy film.
Research shows that the as cast condition product obtained by melting has the natural performance deficiency being difficult to avoid that, such as since heat expansion is cold
Empty caused by contracting, loose and ingredient, nonuniform organization etc..Above-mentioned preparation method needs vacuum, high vacuum environment or lazy
Property gas atmosphere, while the process of material alloys needs high temperature, high instantaneous energy density.In contrast, electro-deposition is
A kind of method for manufacturing thin film at low cost, easy to operate.
It is electrochemical deposition method to prepare the simplest method of high-entropy alloy film.First, electrochemical deposition mild condition, only
It slightly higher need to carry out in room temperature or at room temperature.In addition, electrochemical deposition can be uniformly deposited on various complicated matrixes
On, and can be used for preparing high-entropy alloy film on anisotropic approach.In addition, by controlling electrochemical deposition process condition
(current potential size, pH value, sedimentation time, depositing temperature etc.) can control the element composition and appearance structure of film.2008, in
The Yao Chenzhong of mountain university is successfully electrochemically-deposited in DMF-CH using constant potential3It is high that amorphous amorphous state is prepared in CN systems
Entropy alloy Fe13.8Co28.7Ni4.0Mn22.1 Bi14.9Tm16.5 films.Later, in 2011, Yao Chenzhong et al. is also used
Same mode is prepared for the nanostructure NdFeCoNiMn high-entropy alloy films with soft magnetism.
The plating solution that current electrodeposition process prepares high-entropy alloy film is all made of ionic liquid, DMF-CH3CN(8:2) solvent
System belongs to the organic solvent plating in Non-auqous Solution Electroplating.First, ionic liquid cost it is very high, storage in condition is wanted
Ask high.Secondly, it because the resistance of organic solvent is generally large and metal main salt degree of ionization is not high, therefore often needs to add to improve to lead
The substance of electric energy power.Again, organic solvent is most of inflammable and carries certain toxicity, therefore safety measure is extremely heavy in electroplating process
It wants.Therefore, which is difficult to realize the industrial applications of high-entropy alloy film.
Invention content
It is prepared present invention aim to address electrochemical deposition method and uses organic solvent conduct in high-entropy alloy thin-film process
Economic cost existing for electroplate liquid solvent is high, condition of storage is harsh, needs addition that can improve the substance of conductive capability, organic solvent
It is inflammable, high toxicity, so that the technical issues of being difficult to realize the industrial applications of high-entropy alloy film.
To achieve the goals above, the present invention provides a kind of preparation method of FeCoNiCuMo high-entropy alloys film, with
Deionized water is that solvent is made into electroplate liquid, is made up of electrochemical deposition method；Contain following component in the electroplate liquid：It is soluble
Divalent iron salt, cobalt salt, nickel salt, mantoquita and molybdate, it is trisodium citrate, triethanolamine, glycine, ethylene glycol, anti-oxidant
Agent, additional salt.Wherein, glycine is as brightener；Trisodium citrate and triethanolamine are as complexing agent, ethylene glycol conduct
Enhance the additive of adhesive force；Ascorbic acid is as antioxidant.
Preferably, divalent iron salt, cobalt salt, nickel salt, mantoquita and the molybdate of the solubility are respectively seven hydration sulphur
Sour ferrous iron, cobalt chloride hexahydrate, Nickel dichloride hexahydrate, two Hydrated copper chlorides, Ammonium Molybdate Tetrahydrate, antioxidant is Vitamin C
Acid, additional salt are lithium perchlorate.Each component content is as follows in the electroplate liquid：Green vitriol 4.0-4.5g/L, six water
Close cobalt chloride 3.0-3.5g/L, Nickel dichloride hexahydrate 3.0-3.5g/L, two Hydrated copper chloride 1.0-1.5g/L, Ammonium Molybdate Tetrahydrate
24.0-25.0g/L, trisodium citrate 11.0-12.0g/L, triethanolamine 2.4-2.5mL/L, glycine 0.6-0.7g/L, second two
Alcohol 0.42-0.44mL/L, ascorbic acid 1.0-1.1g/L, lithium perchlorate 3.0-3.5g/L.
Preferably, the preparation method of the FeCoNiCuMo high-entropy alloys film, includes the following steps：
Step S1, three parts of deionized waters are taken, triethanolamine, Ammonium Molybdate Tetrahydrate and mantoquita are dissolved in first part of deionized water
In, obtain solution A；
Step S2, glycine, ethylene glycol, antioxidant, additional salt are dissolved in second part of deionized water, obtain solution B；
Step S3, trisodium citrate, divalent iron salt, cobalt salt, nickel salt are dissolved in third part deionized water, obtain solution C；
Step S4, solution A, solution B and solution C are uniformly mixed, after being aged 1-3h, adjusting mixed solution pH value to 7-8,
It is again heated to 30 DEG C, meanwhile, nitrogen deoxygenation is led into the mixed solution, obtains electroplate liquid；
Step S5, copper-based to be used as cathode using graphite cake as anode, constant potential is electroplated to get to fine and close
FeCoNiCuMo high-entropy alloy films.
It may further be preferable that the step S1 is specially：Take three parts of deionized waters, the total weight of three parts of deionized waters small
In or equal to deionized water total amount needed for electroplate liquid, first triethanolamine is dissolved in first part of deionized water, adds four water
Ammonium molybdate and mantoquita are closed, stirring obtains solution A to dissolving.
It may further be preferable that the step S3 is specially：Trisodium citrate is dissolved in third part deionized water, then is added
Enter divalent iron salt, cobalt salt, nickel salt, stirring and dissolving obtains solution C.
It may further be preferable that the step S4 is specially：Solution A, solution B and solution C are uniformly mixed, added
Ionized water adjusts mixeding liquid volume to target volume, is then aged 1-3h, then adjusts mixed solution pH value to 7-8 using ammonium hydroxide,
Heating water bath is to 30 DEG C again, meanwhile, nitrogen 15min deoxygenations are led into the mixed solution, obtain electroplate liquid；Each group in the electroplate liquid
Divide content as follows：Green vitriol 4.0-4.5g/L, cobalt chloride hexahydrate 3.0-3.5g/L, Nickel dichloride hexahydrate 3.0-
3.5g/L, two Hydrated copper chloride 1.0-1.5g/L, Ammonium Molybdate Tetrahydrate 24.0-25.0g/L, trisodium citrate 11.0-12.0g/
L, triethanolamine 2.4-2.5mL/L, glycine 0.6-0.7g/L, ethylene glycol 0.42-0.44mL/L, ascorbic acid 1.0-1.1g/
L, lithium perchlorate 3.0-3.5g/L.
It may further be preferable that the step S5 is specially：It is copper-based to be used as cathode, permanent electricity using graphite cake as anode
3min is electroplated under the conditions of the 1.1V of position, then takes out, uses ethyl alcohol successively, pure water rinsing is dried to get to fine and close FeCoNiCuMo
High-entropy alloy film.
Nano-titanium dioxide can also be added in the electroplate liquid, nano-titanium dioxide enhancing is prepared
FeCoNiCuMo high-entropy alloy laminated films.
The invention has the beneficial effects that：
High-entropy alloy thin film composition prepared by one, the present invention is uniform, can control thin film composition by adjusting plating solution composition；
Also it can regulate and control film microscopic appearance by heat treatment process；Laminated film can be prepared by adding the nano particles such as titanium dioxide；
It can be prepared in the metal surfaces such as copper, brass, carbon steel, stainless steel, the semiconductor material surfaces such as conductive polymer surfaces and silicon wafer
High-entropy alloy film；The high-entropy alloy film resiativity of preparation is high, and can regulate and control.
Secondly, the present invention by the electrodeposition process of solvent of water prepare high-entropy alloy film, successfully prepare height in aqueous solution
Entropy alloy firm, preparation process temperature is low, energy consumption is small, greatly reduces production cost, and without generating poisonous and harmful substance, tool
Have the characteristics that inexpensive, easily operated and environmentally protective.
Thirdly, method disclosed by the invention have equipment, simple for process, production efficiency is high, production cost is low, safety can
The features such as high by property, is suitable for the industrialized production of high-entropy alloy film.
Description of the drawings
Fig. 1, high-entropy alloy film surface appearance.
Fig. 2, high-entropy alloy film sections pattern.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
The method for preparing the FeCoNiCuMo high-entropy alloy films of the present invention, each component content is such as in the electroplate liquid used
Under：Green vitriol 4.0g/L, cobalt chloride hexahydrate 3.0g/L, Nickel dichloride hexahydrate 3.0g/L, two Hydrated copper chlorides
1.0g/L, Ammonium Molybdate Tetrahydrate 24.0g/L, trisodium citrate 11.0g/L, triethanolamine 2.4mL/L, glycine 0.6g/L, second
Glycol 0.42mL/L, ascorbic acid 1.0g/L, lithium perchlorate 3.0g/L.
Specific preparation method includes the following steps：
Step S1, take the deionized water of three parts of 150mL respectively, first by 1.2mL triethanolamines be dissolved in first part of 150mL go from
In sub- water, two Hydrated copper chloride of 12g Ammonium Molybdate Tetrahydrates and 0.5g is added, stirring obtains solution A to dissolving；
Step S2,0.3g glycine, 0.21mL ethylene glycol, 0.5g ascorbic acid, 1.5g lithium perchlorates are dissolved in second part
In 150mL deionized waters, solution B is obtained；
Step S3,5.5g trisodium citrates are dissolved in third part 150mL deionized waters, it is sub- adds seven hydrated sulfuric acids of 2g
Iron, 1.5g cobalt chloride hexahydrates, 1.5g Nickel dichloride hexahydrates, stirring and dissolving obtain solution C；
Step S4, solution A, solution B and solution C are uniformly mixed, adding deionized water to mixed liquor volume is
500mL, is then aged 1-3h, then adjusts mixed solution pH value to 7 using ammonium hydroxide, then heating water bath is to 30 DEG C, meanwhile, it is mixed to this
It closes and leads to nitrogen 15min deoxygenations in solution, obtain electroplate liquid；
Step S5, copper-based to be used as cathode using graphite cake as anode, 3min is electroplated under the conditions of constant potential 1.1V, then
It takes out, uses ethyl alcohol, pure water rinsing successively, dry to get to fine and close FeCoNiCuMo high-entropy alloy films.
Embodiment 2
The method for preparing the FeCoNiCuMo high-entropy alloy films of the present invention, each component content is such as in the electroplate liquid used
Under：Green vitriol 4.5g/L, cobalt chloride hexahydrate 3.5g/L, Nickel dichloride hexahydrate 3.5g/L, two Hydrated copper chlorides
1.5g/L, Ammonium Molybdate Tetrahydrate 25.0g/L, trisodium citrate 12.0g/L, triethanolamine 2.5mL/L, glycine 0.7g/L, second
Glycol 0.44mL/L, ascorbic acid 1.1g/L, lithium perchlorate 3.5g/L.
Specific preparation method includes the following steps：
Step S1, the deionized water of three parts of 150mL is taken to be contained in three beakers respectively, it is first that 1.25mL triethanolamines is molten
In first part of 150mL deionized water, two Hydrated copper chloride of 12.5g Ammonium Molybdate Tetrahydrates and 0.75g is added, is stirred to molten
Solution, obtains solution A；
Step S2,0.35g glycine, 0.22mL ethylene glycol, 0.55g ascorbic acid, 1.75g lithium perchlorates are dissolved in second
In part 150mL deionized waters, solution B is obtained；
Step S3,6g trisodium citrates are dissolved in third part 150mL deionized waters, add seven hydrated sulfuric acids of 2.25g
Ferrous iron, 1.75g cobalt chloride hexahydrates, 1.75g Nickel dichloride hexahydrates, stirring and dissolving obtain solution C；
Step S4, solution A, solution B and solution C are transferred in 500mL volumetric flasks, 500mL are settled to deionized water,
Then it is aged 1-3h, then mixed solution pH value is adjusted to 7.5 using ammonium hydroxide, then heating water bath is to 30 DEG C, meanwhile, it is molten to the mixing
Lead to nitrogen 15min deoxygenations in liquid, obtains electroplate liquid；
Step S5, copper-based to be used as cathode using graphite cake as anode, 3min is electroplated under the conditions of constant potential 1.1V, then
It takes out, uses ethyl alcohol, pure water rinsing successively, dry to get to fine and close FeCoNiCuMo high-entropy alloy films.It is prepared by the embodiment
The surface topographies of FeCoNiCuMo high-entropy alloy films see that Fig. 1, Cross Section Morphology are shown in Fig. 2.Film is by micron as seen from the figure
Grade microballoon is constituted, and membrane structure even compact is tightly combined with matrix.
Embodiment 3
The method for preparing the FeCoNiCuMo high-entropy alloy films of the present invention, each component content is such as in the electroplate liquid used
Under：Green vitriol 4.2g/L, cobalt chloride hexahydrate 3.3g/L, Nickel dichloride hexahydrate 3.2g/L, two Hydrated copper chlorides
1.2g/L, Ammonium Molybdate Tetrahydrate 24.0g/L, trisodium citrate 11.0g/L, triethanolamine 2.4mL/L, glycine 0.7g/L, second
Glycol 0.44mL/L, ascorbic acid 1.1g/L, lithium perchlorate 3.0g/L, nano-titanium dioxide 0-20g/L.
Specific preparation method includes the following steps：
Step S1, the deionized water of three parts of 150mL is taken to be contained in three beakers respectively, it is first that 1.2mL triethanolamines is molten
In first part of 150mL deionized water, two Hydrated copper chloride of 12g Ammonium Molybdate Tetrahydrates and 0.6g is added, stirring is obtained to dissolving
To solution A；
Step S2,0.35g glycine, 0.22mL ethylene glycol, 0.55g ascorbic acid, 1.5g lithium perchlorates are dissolved in second
In part 150mL deionized waters, solution B is obtained；
Step S3,5.5g trisodium citrates are dissolved in third part 150mL deionized waters, add seven hydrated sulfuric acids of 2.1g
Ferrous iron, 1.65g cobalt chloride hexahydrates, 1.6g Nickel dichloride hexahydrates, stirring and dissolving obtain solution C；
Step S4, solution A, solution B and solution C are transferred in 500mL volumetric flasks, nano-titanium dioxide is added, spends
Ionized water is settled to 500mL, is then aged 1-3h, then adjusts mixed solution pH value to 8 using ammonium hydroxide, then heating water bath is to 30
DEG C, meanwhile, nitrogen 15min deoxygenations are led into the mixed solution, obtain electroplate liquid；
Step S5, copper-based to be used as cathode using graphite cake as anode, 3min is electroplated under the conditions of constant potential 1.1V, then
It takes out, uses ethyl alcohol, pure water rinsing successively, dry enhances FeCoNiCuMo high-entropy alloys to get to fine and close nano-titanium dioxide
Laminated film.
In conclusion the present invention provides a kind of methods preparing high-entropy alloy film as the electrodeposition process of solvent using water.
This method is nontoxic using water as solvent, and manufacturing cost is cheap, have equipment, simple for process, production efficiency is high, safety can
The features such as high by property, is suitable for the industrialized production of high-entropy alloy film.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, according to the technical essence of the invention
To any simple modification, equivalent change and modification made by above example, in the range of still falling within technical solution of the present invention.
Claims (9)
1. a kind of preparation method of FeCoNiCuMo high-entropy alloys film, which is characterized in that be made into electricity by solvent of deionized water
Plating solution is made up of electrochemical deposition method；The electroplate liquid includes following component：Divalent iron salt, cobalt salt, the nickel of solubility
Salt, mantoquita and molybdate, trisodium citrate, triethanolamine, glycine, ethylene glycol, antioxidant, additional salt.
2. the preparation method of FeCoNiCuMo high-entropy alloys film as described in claim 1, which is characterized in that the solubility
Divalent iron salt, cobalt salt, nickel salt, mantoquita and molybdate be respectively green vitriol, cobalt chloride hexahydrate, six hydration chlorine
Change nickel, two Hydrated copper chlorides, Ammonium Molybdate Tetrahydrate, antioxidant is ascorbic acid, and additional salt is lithium perchlorate.
3. the preparation method of FeCoNiCuMo high-entropy alloys film as claimed in claim 2, which is characterized in that the electroplate liquid
Middle each component content is as follows：Green vitriol 4.0-4.5g/L, cobalt chloride hexahydrate 3.0-3.5g/L, Nickel dichloride hexahydrate
3.0-3.5g/L, two Hydrated copper chloride 1.0-1.5g/L, Ammonium Molybdate Tetrahydrate 24.0-25.0g/L, trisodium citrate 11.0-
12.0g/L, triethanolamine 2.4-2.5mL/L, glycine 0.6-0.7g/L, ethylene glycol 0.42-0.44mL/L, ascorbic acid 1.0-
1.1g/L, lithium perchlorate 3.0-3.5g/L.
4. the preparation method of the FeCoNiCuMo high-entropy alloy films as described in claim 1-3 any one, which is characterized in that
Include the following steps：
S1, three parts of deionized waters are taken, triethanolamine, Ammonium Molybdate Tetrahydrate and mantoquita is dissolved in first part of deionized water, obtained
Solution A；
S2, glycine, ethylene glycol, antioxidant, additional salt are dissolved in second part of deionized water, obtain solution B；
S3, trisodium citrate, divalent iron salt, cobalt salt, nickel salt are dissolved in third part deionized water, obtain solution C；
S4, solution A, solution B and solution C are uniformly mixed, after being aged 1-3h, adjust mixed solution pH value to 7-8, be again heated to
30 DEG C, meanwhile, nitrogen deoxygenation is led into the mixed solution, obtains electroplate liquid；
S5, using graphite cake as anode, copper-based to be used as cathode, constant potential is electroplated to get to fine and close FeCoNiCuMo
High-entropy alloy film.
5. the preparation method of FeCoNiCuMo high-entropy alloys film as claimed in claim 4, which is characterized in that the step S1
Specially：Three parts of deionized waters, the total weight of three parts of deionized waters are taken to be less than or equal to the deionized water total amount needed for electroplate liquid,
First triethanolamine is dissolved in first part of deionized water, adds Ammonium Molybdate Tetrahydrate and mantoquita, stirring obtains solution to dissolving
A。
6. the preparation method of FeCoNiCuMo high-entropy alloys film as claimed in claim 5, which is characterized in that the step S3
Specially：Trisodium citrate is dissolved in third part deionized water, divalent iron salt, cobalt salt, nickel salt are added, stirring and dissolving obtains
To solution C.
7. the preparation method of FeCoNiCuMo high-entropy alloys film as claimed in claim 6, which is characterized in that the step S4
Specially：Solution A, solution B and solution C are uniformly mixed, deionized water is added and adjusts mixeding liquid volume to target volume, so
After be aged 1-3h, then mixed solution pH value is adjusted to 7-8 using ammonium hydroxide, then heating water bath is to 30 DEG C, meanwhile, to the mixed solution
In lead to nitrogen 15min deoxygenations, obtain electroplate liquid；Each component content is as follows in the electroplate liquid：Green vitriol 4.0-4.5g/
L, cobalt chloride hexahydrate 3.0-3.5g/L, Nickel dichloride hexahydrate 3.0-3.5g/L, two Hydrated copper chloride 1.0-1.5g/L, four hydrations
Ammonium molybdate 24.0-25.0g/L, trisodium citrate 11.0-12.0g/L, triethanolamine 2.4-2.5mL/L, glycine 0.6-0.7g/
L, ethylene glycol 0.42-0.44mL/L, ascorbic acid 1.0-1.1g/L, lithium perchlorate 3.0-3.5g/L.
8. the preparation method of FeCoNiCuMo high-entropy alloys film as claimed in claim 7, which is characterized in that the step S5
Specially：It is copper-based to be used as cathode using graphite cake as anode, 3min is electroplated under the conditions of constant potential 1.1V, then takes out, successively
With ethyl alcohol, pure water rinsing, dry to get to fine and close FeCoNiCuMo high-entropy alloy films.
9. the preparation method of FeCoNiCuMo high-entropy alloys film as claimed in claim 7, which is characterized in that by described
Nano-titanium dioxide is added in electroplate liquid, nano-titanium dioxide enhancing FeCoNiCuMo high-entropy alloy laminated films are prepared.
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