CN104294327A - Ionic liquid electrolyte and method for preparing bright aluminum coating by use of ionic liquid electrolyte - Google Patents
Ionic liquid electrolyte and method for preparing bright aluminum coating by use of ionic liquid electrolyte Download PDFInfo
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Abstract
The invention provides an ionic liquid electrolyte and a method for preparing a bright aluminum coating by use of the ionic liquid electrolyte, and mainly aims at solving the problems of inappropriate viscosity, electrical conductivity and the like of the existing ionic liquid for preparing the bright aluminum coating. The electrolyte is composed of an ionic liquid, an anhydrous aluminum halide salt and auxiliaries, wherein the molar ratio of the ionic liquid to the anhydrous aluminum halide salt is 1: (1.5-2.0), and the molar ratio of the ionic liquid to the auxiliaries is 1: (0.1-4). The method for preparing the bright aluminum coating by use of the ionic liquid electrolyte comprises the following steps: firstly, putting an electrolyzer in a nitrogen or argon environment atmosphere without water or oxygen under normal pressure, adding the ionic liquid electrolyte, and performing electrolysis under the conditions of an electrolysis temperature of 10-30 DEG C, the current density of 1-10A/dm<2> and regulated electrolyzer pressure, thereby obtaining the bright luster aluminum coating. After the auxiliaries are added to the ionic liquid electrolyte for preparing the bright aluminum coating, the electrolyzer pressure is reduced and the viscosity and the electrical conductivity of the ionic liquid are improved, and therefore, the electrolytic deposited bright aluminum coating is obtained.
Description
Technical field
The present invention relates to a kind of il electrolyte and prepare the method for bright aluminium coat with this electrolytic solution, belong to field of electroplating.
Background technology
Because aluminium belongs to the electropotential cathodic metal more negative than hydrogen, aqueous systems electrolytic aluminum can not realize, and high temperature fused salt electrolysis aluminum technology temperature is high, directly can not obtain solid aluminum.The appearance of low-temperature electrolytic aluminum technology and be applied as electrolytic process and directly obtain solid aluminum product and provide possibility.The electrolytic aluminum of low temperature non-aqueous system mainly includes machine solvent system, molten salt system and ion liquid system.Comparatively speaking, the advantage of ion liquid system is that temperature use range is wide, have higher specific conductivity and wider electrochemical window, and side reaction is few, non-volatile, nonflammable.Current employing ion liquid system galvanic deposit obtains research paper and the common report of patent of metal aluminum or aluminum alloy, system positively charged ion relates generally to imidazole salts, pyridinium salt, pyrroles's salt, piperidinium salt, quaternary ammonium salt, dimethyl sulfone etc., and negatively charged ion comprises halide anion, tetrafluoroborate, [N (CF
3sO
2)
2]
-deng.For maximum in electric deposition aluminum research be chloro-aluminate system, its good physico-chemical property, lower viscosity and electrolysis temperature are that electrolytic aluminum provides a kind of desirable room temperature reaction medium, become the preferred electrolyte system of low-temperature electrolytic aluminium.Nonetheless, there is the problems such as coating is loose, dendrite in the interface control process still showing as concentration polarization of chloro-aluminate system electric deposition aluminum.The aluminium coat obtaining fine and close light not only can improve the attractive appearance of plated item, and can also increase its barrier propterty to matrix, be one of important directions of Electroplating Aluminum research always.For chloro-aluminate electrolytic aluminum system, increase the electrochemical reaction polarization of deposition surface or reduce by two kinds of effective ways that electrolytical concentration polarization is the fine and close smooth aluminium coat of acquisition.Although suitably improve electrodeposition temperature, viscosity of il can be made to decline, ion diffuse speed is accelerated, but the chemical reaction of electrode surface is accelerated gradient and is greater than ion migration quickening gradient, thus exacerbate concentration polarization, moreover there is thermolability during glyoxaline ion liquid high temperature, this method is also inadvisable.Chinese patent CN101760758A, while electric deposition aluminum, makes electrolyzer centrifugal rotation produce super gravity field, strengthening convection current and diffusion process, can crystal grain thinning, avoid the generation of dendrite aluminium, but production unit conditional request is high, belongs to the metal electrodeposition field under special conditions.The organic solvent that US Patent No. 2013168258A1 adopts specific inductivity to be less than or equal to 8 improves the electroconductibility of electrolytic solution as hexane, toluene, Anaesthetie Ether, ethyl acetate etc. and obtains the aluminium coat of continuous uniform, but these organic solvents are inflammable and explosive, add the danger of application.US Patent No. 20120006688A1 adopts following three compounds as additive,
r
3n
+(R
4)
3hal
-, R
5sO
3 -m
+, can obtain the aluminium coat of smooth densification in the process of various types of electrolyzing aluminum from ionic liquid, not mentioned additive is on the impact of electrolytic conductivity, viscosity.Chinese patent CN103849911A, by adding 0.5-15g/L pyridine derivate, produces electrode surface absorption and increases electrode surface chemical polarization, thus obtaining bright aluminium coat, but also increases groove pressure simultaneously, reduces current density.Although various light or technology of all aluminizing respectively have its features and application, we still need constantly to inquire into new Method and Technology and obtain excellent aluminium coat.
In addition, when the plated item obtained or electroplanting device in the end arrange and clean, to adopt ethanol, acetone equal solvent habitually in the past, but these dissolvings are not only inflammable and explosive, also produce bonding with the active aluminum ion in electrolytic solution, cause product not wash clean clearly, scavenging solution viscosity increases, so that thickness cannot use, need a kind of solvent of not having an effect with chloro-aluminate system zwitterion or clean-out system.
Summary of the invention
The present invention is for the purpose of solving the problem, and propose a kind of il electrolyte and prepare the method for bright aluminium coat with this electrolytic solution, this il electrolyte is at ionic liquid-anhydrous aluminum halide salt AlX
3auxiliary agent is added in system, the interpolation of auxiliary agent improves viscosity of il and specific conductivity, thus obtaining galvanic deposit light aluminium coat, this auxiliary agent also can be used for the dilution, product cleaning etc. of chlorine aluminic acid type Electroplating Aluminum electrolytic solution, and waste liquid distillation can be reused after collecting.
For achieving the above object, the present invention adopts following technical proposals:
A kind of il electrolyte, by ionic liquid, anhydrous aluminum halide salt (AlX
3) and auxiliary agent composition; The positively charged ion of above-mentioned ionic liquid is imidazoles, pyridines, quaternary amines ， quaternary phosphine class, pyroles, piperidines, and morpholine class and dimethyl sulfone or their mixture, negatively charged ion is halogen, above-mentioned anhydrous aluminum halide salt (AlX
3) X be Cl, Br or I, above-mentioned auxiliary agent is haloalkane, is methylene dichloride, trichloromethane, methylene bromide, halothane or their isomers.
The mol ratio of described ionic liquid and anhydrous aluminum halide salt is 1:1.5-2.0, and the mol ratio of ionic liquid and auxiliary agent is 1:0.1-4.
The preparation of above-mentioned il electrolyte is in the nitrogen or argon ambient atmosphere of normal pressure anhydrous and oxygen-free, under water-content, oxygen level condition all≤5 ‰, by described ionic liquid and anhydrous aluminum halide salt (AlX
3) by above-mentioned mixed in molar ratio, and then in mixed solution, add the auxiliary agent of above-mentioned mol ratio.
The method of bright aluminium coat is prepared with this electrolytic solution, its preparation method comprises the steps: the nitrogen or the argon ambient atmosphere that first electrolyzer are placed in normal pressure anhydrous and oxygen-free, water-content, oxygen level all≤5 ‰, by described ionic liquid and anhydrous aluminum halide salt (AlX in above-mentioned electrolyzer
3) mix in molar ratio, and then in mixed solution, add the auxiliary agent of above-mentioned mol ratio, anode adopts active anode fine aluminium or inert anode glass carbon, negative electrode is conducting metal matrix, at electrolysis temperature 10-30 DEG C, use soluble anode groove pressure-controlled scope 0.5-1.5V, use inert anode groove pressure-controlled scope 2.5-4.0V, current density 1-10A/dm
2condition under then carry out electrolysis 3-20min, obtain the aluminium coat of specular gloss.
The described method preparing bright aluminium coat with this electrolytic solution, its specific implementation step is as follows:
A, nitrogen electrolyzer being placed in normal pressure anhydrous and oxygen-free or argon ambient atmosphere, water-content, oxygen level are all≤5 ‰;
B, get each composition of above-mentioned il electrolyte in molar ratio, first in electrolyzer, ionic liquid is mixed with anhydrous aluminum halide salt, add auxiliary agent wherein again, anode can adopt active anode fine aluminium or inert anode glass carbon, negative electrode is conducting metal matrix, as metal or their alloys such as the copper sheet after sanding and polishing, titanium sheet, stainless steel substrates, zinc metal sheets, pole span 5-30mm; If employing inert anode, the content of anhydrous aluminum halide salt can reduce gradually along with the deposition of aluminium and the generation of halogen simple substance, preferably adds at any time to maintain the carrying out of electrolysis and the quality of al deposition layer.
C, electrolysis temperature should control below auxiliary agent boiling temperature, between 10-30 DEG C, use soluble anode groove pressure-controlled scope 0.5-1.5V, use inert anode groove pressure-controlled scope 2.5-4.0V, current density 1-10A/dm
2condition under carry out electrolysis, obtained bright aluminium coat;
D, take out the aluminium plating sheet of above-mentioned bright aluminium coat, put into above-mentioned auxiliary agent cleaning three times, seasoning, seals up for safekeeping, uses auxiliary agent repeatedly to concentrate distilation to recycle.
The invention has the beneficial effects as follows: the auxiliary agent in il electrolyte of the present invention by improving viscosity of il and specific conductivity, thus obtains galvanic deposit light aluminium coat, and can be used for dilution, the cleaning of il electrolyte.Adopt room temperature chlorine aluminic acid type ionic liquid, add appropriate electrolytic solution auxiliary agent, be mixed with electrolytic solution, adding of auxiliary agent, the viscosity of electrolytic solution can be significantly reduced, improve the specific conductivity of electrolytic solution, reduce concentration polarization to impacts such as coarse, the dendrite that settled layer causes.This auxiliary agent also can be used for the dilution, product cleaning etc. of chlorine aluminic acid type Electroplating Aluminum electrolytic solution, and waste liquid distillation can be reused after collecting.Auxiliary agent low toxicity, non-combustible, use simple, cheap.
In addition, after il electrolyte adds auxiliary agent, electrolyzer pressure drop is low, drastically increase current density during electrolysis, shorten the electroplating time obtaining same thickness aluminium coat, grain refining when making al deposition, smooth, can reach gloss as minute surface, the al deposition layer of acquisition has modification, protective effect.
Figure of description
Fig. 1 be 1-methyl-3 butyl imidazole villaumite in the present invention and methylene dichloride mol ratio 1:3 time carry out the bright coating picture of electrolysis acquisition;
Fig. 2 is that electrolysis of the present invention is not by adding the SEM image of the aluminium coat of methylene dichloride during electricity 16.2C;
Fig. 3 is that electrolysis of the present invention is by adding the aluminium plated surface SEM image after methylene dichloride by 1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) and methylene dichloride 1:3 mol ratio during electricity 16.2C;
Fig. 4 is that methylene dichloride content in intermediate ion liquid electrolyte of the present invention is on the impact of specific conductivity;
Fig. 5 is that methylene dichloride content in intermediate ion liquid electrolyte of the present invention is on the impact of viscosity.
Embodiment
Embodiment 1
A kind of il electrolyte, by ionic liquid, anhydrous aluminum halide salt AlX
3and auxiliary agent composition; Above-mentioned ionic liquid and anhydrous aluminum halide salt AlX
3for 1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) and anhydrous AlCl
3, above-mentioned auxiliary agent is methylene dichloride;
Described 1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) and anhydrous AlCl
3molar ratio be 1:2,1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) with the molar ratio of methylene dichloride be 1:3.
The method of bright aluminium coat is prepared with this electrolytic solution, its preparation method comprises the steps: the nitrogen or the argon ambient atmosphere that first electrolyzer are placed in normal pressure anhydrous and oxygen-free, water-content, oxygen level are all≤5 ‰, each one-tenth getting above-mentioned il electrolyte by above-mentioned mol ratio is placed in above-mentioned electrolyzer, anode adopts active anode fine aluminium or inert anode glass carbon, negative electrode is conducting metal matrix, then carries out electrolysis, obtains the aluminium coat of specular gloss.
Prepare the method for bright aluminium coat with this electrolytic solution, its specific implementation step is as follows:
First in the nitrogen or argon ambient atmosphere of normal pressure anhydrous and oxygen-free (water-content, oxygen level are all≤5 ‰), can choice for use glove box.Each one-tenth getting above-mentioned il electrolyte by above-mentioned mol ratio is placed in electrolyzer, is mixed with il electrolyte, and Conductivity Ratio improves 2.7 times before not adding auxiliary agent, and viscosity ratio declines 6 times before not adding auxiliary agent.After sanding and polishing, copper sheet is as negative electrode, and high-purity aluminium flake is anode, and two pole distances keep 10mm, and temperature controls at 30 DEG C.Use constant voltage dc source, adjustment tank pressure 0.6v, current density can reach 2.5A/dm
2, improve 10 times than before non-adding assistant.Plating 10min, obtains the aluminium coat of specular gloss.As shown in Figure 1, white wire frame inner compartment is that light is aluminized sheet, and the visible character pattern mapped, to show the visual perception of specular gloss.Scanning electron microscope is adopted to scan electroplating the sheet of aluminizing obtained, as Fig. 2-3, under identical magnification (20,000 times), Fig. 2 is the microscopic appearance of the aluminium plated surface not adding methylene dichloride, the large surface irregularity of crystal grain, Fig. 3 adds the microscopic appearance of the aluminium plated surface after methylene dichloride for press 1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) and methylene dichloride 1:3 mol ratio, the obvious refinement of particle, smooth.
Taking-up is aluminized sheet, and put into methylene dichloride cleaning three times, seasoning, seals up for safekeeping.Clean-out system is repeatedly used to concentrate distilation to recycle.
Embodiment 2
A kind of il electrolyte, by ionic liquid, anhydrous aluminum halide salt AlX
3and auxiliary agent composition; Above-mentioned ionic liquid and anhydrous aluminum halide salt AlX
3for 1-methyl-3 ethyl imidazol(e) villaumite ([EMIM] Cl) and anhydrous AlCl
3, above-mentioned auxiliary agent is methylene dichloride;
Described 1-methyl-3 ethyl imidazol(e) villaumite ([EMIM] Cl) and anhydrous AlCl
3molar ratio be 1:2,1-methyl-3 ethyl imidazol(e) villaumite ([EMIM] Cl) with the molar ratio of methylene dichloride be 1:3.
The method of bright aluminium coat is prepared with this electrolytic solution, its preparation method comprises the steps: the nitrogen or the argon ambient atmosphere that first electrolyzer are placed in normal pressure anhydrous and oxygen-free, water-content, oxygen level are all≤5 ‰, each one-tenth getting above-mentioned il electrolyte by above-mentioned mol ratio is placed in above-mentioned electrolyzer, anode adopts active anode fine aluminium or inert anode glass carbon, negative electrode is conducting metal matrix, then carries out electrolysis, obtains the aluminium coat of specular gloss.
Prepare the method for bright aluminium coat with this electrolytic solution, its specific implementation step is as follows:
First in the nitrogen or argon ambient atmosphere of normal pressure anhydrous and oxygen-free (water-content, oxygen level are all≤5 ‰), can choice for use glove box.Each one-tenth getting above-mentioned il electrolyte by above-mentioned mol ratio is placed in electrolyzer, and be mixed with il electrolyte, specific conductivity is 2.5 times before not adding auxiliary agent, and viscosity ratio declines 5.1 times before not adding auxiliary agent.After sanding and polishing, copper sheet is as negative electrode, and noble electrode glass carbon is anode, and two pole distances keep 10mm, and temperature controls at 30 DEG C.Use constant voltage dc source, adjustment tank pressure 3.0v, current density can reach 5A/dm
2, improve 8 times than before non-adding assistant.Plating 5min, obtains the aluminium coat of specular gloss.Taking-up is aluminized sheet, and put into methylene dichloride cleaning three times, seasoning, seals up for safekeeping.Clean-out system is repeatedly used to concentrate distilation to recycle.
Embodiment 3
A kind of il electrolyte, by ionic liquid, anhydrous aluminum halide salt AlX
3and auxiliary agent composition; Above-mentioned ionic liquid and anhydrous aluminum halide salt AlX
3for 1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) and anhydrous AlCl
3, above-mentioned auxiliary agent is trichloromethane.
Described 1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) and anhydrous AlCl
3molar ratio be 1:2,1-methyl-3 butyl imidazole villaumite ([BMIM] Cl) with the molar ratio of trichloromethane be 1:3.
The method of bright aluminium coat is prepared with this electrolytic solution, its preparation method comprises the steps: the nitrogen or the argon ambient atmosphere that first electrolyzer are placed in normal pressure anhydrous and oxygen-free, water-content, oxygen level are all≤5 ‰, each one-tenth getting above-mentioned il electrolyte by above-mentioned mol ratio is placed in above-mentioned electrolyzer, anode adopts active anode fine aluminium or inert anode glass carbon, negative electrode is conducting metal matrix, then carries out electrolysis, obtains the aluminium coat of specular gloss.
Prepare the method for bright aluminium coat with this electrolytic solution, its specific implementation step is as follows:
First in the nitrogen or argon ambient atmosphere of normal pressure anhydrous and oxygen-free (water-content, oxygen level are all≤5 ‰), can choice for use glove box.Each one-tenth getting above-mentioned il electrolyte by above-mentioned mol ratio is placed in electrolyzer, and be mixed with il electrolyte, specific conductivity is 1.6 times before not adding auxiliary agent, and viscosity ratio declines 42% before not adding auxiliary agent.After sanding and polishing, copper sheet is as negative electrode, and high-purity aluminium flake is anode, and two pole distances keep 10mm, and temperature controls at 20 DEG C.Use pulse plating power, adjustment tank pressure 0.7v, current density can reach 1.2A/dm
2, improve 10 times than before non-adding assistant.Plating 20min, obtains argenteous aluminium coat.Taking-up is aluminized sheet, and put into trichloromethane cleaning three times, seasoning, seals up for safekeeping.Clean-out system is repeatedly used to concentrate distilation to recycle.
The interpolation of described auxiliary agent, can significantly reduce the viscosity of electrolytic solution, improves the specific conductivity of electrolytic solution, reduces concentration polarization to impacts such as coarse, the dendrite that settled layer causes.As shown in Figure 4, with [BMIM] Cl for radix, methylene dichloride accounts for [BMIM] Cl mole number within the scope of 0-77.6%, account for the increase of addition with methylene dichloride, electrolytic conductivity increases; Methylene dichloride accounts for [BMIM], and Cl mole number is greater than after 77.6%, and account for the increase of addition with methylene dichloride, electrolytic conductivity declines gradually; As shown in Figure 5, with [BMIM] Cl for radix, methylene dichloride accounts for [BMIM] Cl mole number within the scope of 0-80%, account for the increase of addition with methylene dichloride, electrolytic solution viscosity declines gradually.
Claims (5)
1. an il electrolyte, is characterized in that, by ionic liquid, and anhydrous aluminum halide salt AlX
3and auxiliary agent composition; The positively charged ion of above-mentioned ionic liquid is imidazoles, pyridines, quaternary amines ， quaternary phosphine class, pyroles, piperidines, and morpholine class and dimethyl sulfone or their mixture, negatively charged ion is halogen, above-mentioned anhydrous aluminum halide salt AlX
3x be Cl, Br or I, above-mentioned auxiliary agent is haloalkane, is methylene dichloride, trichloromethane, methylene bromide, halothane or their isomers.
2. a kind of il electrolyte as claimed in claim 1, is characterized in that, the mol ratio of described ionic liquid and anhydrous aluminum halide salt is 1:1.5-2.0, and the mol ratio of ionic liquid and auxiliary agent is 1:0.1-4.
3. a kind of il electrolyte as claimed in claim 1, it is characterized in that, the preparation of described il electrolyte is in the nitrogen or argon ambient atmosphere of normal pressure anhydrous and oxygen-free, under water-content, oxygen level condition all≤5 ‰, by described ionic liquid and anhydrous aluminum halide salt AlX
3by described mixed in molar ratio, and then in mixed solution, add the auxiliary agent of described mol ratio.
4. the method for bright aluminium coat is prepared by il electrolyte according to claim 1, it is characterized in that, first electrolyzer is placed in nitrogen or the argon ambient atmosphere of normal pressure anhydrous and oxygen-free, water-content, oxygen level all≤5 ‰, by described ionic liquid and anhydrous aluminum halide salt AlX in above-mentioned electrolyzer
3mix in molar ratio, and then in mixed solution, add the auxiliary agent of above-mentioned mol ratio, anode adopts active anode fine aluminium or inert anode glass carbon, negative electrode is conducting metal matrix, at electrolysis temperature 10-30 DEG C, use soluble anode groove pressure-controlled scope 0.5-1.5V, use inert anode groove pressure-controlled scope 2.5-4.0V, current density 1-10A/dm
2condition under then carry out electrolysis, obtain the aluminium coat of specular gloss.
5. il electrolyte as claimed in claim 4 prepares the method for bright aluminium coat, and its specific implementation step is as follows:
A, nitrogen electrolyzer being placed in normal pressure anhydrous and oxygen-free or argon ambient atmosphere, water-content, oxygen level are all≤5 ‰;
B, get each component of il electrolyte in molar ratio, first in electrolyzer, ionic liquid is mixed with anhydrous aluminum halide salt, add auxiliary agent wherein again, anode can adopt active anode fine aluminium or inert anode glass carbon, negative electrode is conducting metal matrix, as metal or their alloys such as the copper sheet after sanding and polishing, titanium sheet, stainless steel substrates, zinc metal sheets, pole span 5-30mm;
C, electrolysis temperature should control below auxiliary agent boiling temperature, between 10-30 DEG C, use soluble anode groove pressure-controlled scope 0.5-1.5V, use inert anode groove pressure-controlled scope 2.5-4.0V, current density 1-10A/dm
2condition under carry out electrolysis 3-20min, obtained bright aluminium coat;
D, take out the aluminium plating sheet of above-mentioned bright aluminium coat, put into above-mentioned auxiliary agent cleaning three times, seasoning, seals up for safekeeping, uses auxiliary agent repeatedly to concentrate distilation to recycle.
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| CN111321427A (en) * | 2020-03-05 | 2020-06-23 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
| CN115161733A (en) * | 2022-09-08 | 2022-10-11 | 苏州优缘建材有限公司 | Surface treatment structure of aluminum alloy and preparation method thereof |
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| CN105671605A (en) * | 2015-12-28 | 2016-06-15 | 银邦金属复合材料股份有限公司 | Manufacturing method for single-side-aluminum-coated steel plates |
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| CN111321427A (en) * | 2020-03-05 | 2020-06-23 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
| CN111321427B (en) * | 2020-03-05 | 2021-05-28 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
| CN115161733A (en) * | 2022-09-08 | 2022-10-11 | 苏州优缘建材有限公司 | Surface treatment structure of aluminum alloy and preparation method thereof |
| CN115161733B (en) * | 2022-09-08 | 2022-12-13 | 苏州优缘建材有限公司 | Surface treatment structure of aluminum alloy and preparation method thereof |
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