CN104878408A - Method for directly electrodepositing zinc oxide to prepare micro-nano zinc layer at low temperature - Google Patents
Method for directly electrodepositing zinc oxide to prepare micro-nano zinc layer at low temperature Download PDFInfo
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- CN104878408A CN104878408A CN201510273097.8A CN201510273097A CN104878408A CN 104878408 A CN104878408 A CN 104878408A CN 201510273097 A CN201510273097 A CN 201510273097A CN 104878408 A CN104878408 A CN 104878408A
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Abstract
The invention discloses a method for directly electrodepositing zinc oxide to prepare a micro-nano zinc layer at a low temperature. The method comprises the following steps: adopting zinc oxide powder (analytical reagent) as a raw material; adopting choline chloride/urea (the molar ratio is 1:2) ionic liquid as an electrolyte; adding excess zinc oxide powder into the ionic liquid, and stirring for 10 hours at the constant temperature of 60-100 DEG C to form a saturated electrolyte solution containing zinc oxide; carrying out electro-deposition by adopting a three-electrode system, namely, a discal platinum electrode is adopted as a counter electrode, to-be-plated metallic matrixes such as a polished copper sheet is a working electrode or a cathode, and a silver electrode is adopted as a reference electrode, wherein the electro-deposition reaction is carried out for 25-60 minutes at the temperature of 40-100 DEG C and under the condition of minus 1.4-minus 1.7 V. According to the method, the reaction temperature, the electrode potential, and the deposition time are controlled, so that the characteristics like the appearance of the micro-nano zinc metal layer can be regulated and controlled; the method has the advantages of being high in efficiency, low in energy consumption, low in raw material price, free of pollution, and the like, and belongs to the technical field of green electro-deposition technologies.
Description
Technical field
The present invention relates to a kind of method being prepared micro-nano zinc layers under low temperature by the direct galvanic deposit of zinc oxide, belong to green electrodeposition technology technical field.
Background technology
China is the maximum countries of zinc reserves, and from 1992, China's zinc output ranked first in the world, and metallic zinc, as the base mateiral of industrial society, is widely used in every field.Modern zinc metallurgy is mainly divided into pyrometallurgy of zinc and zinc hydrometallurgy, zinc hydrometallurgy due to its comprehensive resource utilization rate high, the advantages such as power consumption is relatively low, become the Main way of current zinc Metallurgical Industry Development.Wherein, electro-galvanizing process is last procedure of zinc hydrometallurgy, and the zinc-plated method of traditional electrical is carried out in water solution system, and wherein the compactness, luminance brightness etc. of generation to metal plating of hydrogen evolution phenomenon have a significant impact.The zinc-plated needs of traditional electrical strictly control the potential of hydrogen of the aqueous solution, the generation of phenomenon that the moment watches out for " liberation of hydrogen ".In addition, the electrochemical window of the aqueous solution is narrower, and the hydrogen produced in electrodeposition process can produce hydrogen embrittlement harm to matrix, and the plating solution of electrodepositing zinc the reason such as to be easily oxidized and to also limit its application.Ionic liquid is that a kind of room temperature be made up of ion completely melts salt.Compared with the aqueous solution, ionic liquid has that electrochemical window is wide, chemical heat stability is high, specific conductivity is high, steam forces down, non-combustible, and environmental protection, the excellent characteristics such as repeatedly can to recycle.Wherein choline chloride 60 class ionic liquid is due to advantages such as its economy, added value are high, recoverables, more and more receives the concern of people, and is applied to various electrodeposition gradually.At present, the galvanic deposit of Metals in Ionic Liquids zinc mainly adopts zinc chloride to be raw material, but the toxic gas chlorine that deposition process produces causes certain corrosion to equipment etc.Therefore, the research preparing metallic zinc by cheap, free of contamination zinc oxide as the direct galvanic deposit of presoma starts rapidly.
Summary of the invention
The present invention is directed to the technical problem that the existence of metallic zinc process is prepared in current galvanic deposit, there is provided a kind of method being prepared micro-nano zinc coating in ionic liquid at low temperatures by the direct galvanic deposit of zinc oxide, the inventive method has the features such as process control, efficiency is high, with low cost, energy consumption is low.
For reach foregoing invention create object, the present invention by the following technical solutions:
The method preparing micro-nano zinc layers by the direct galvanic deposit of zinc oxide under a kind of low temperature of the present invention is characterized in that having following process and step:
A. the preparation of choline chloride/urea ionic liquid: with choline chloride 60 and urea for initial feed, 1:2 mixes in molar ratio, at 80 DEG C constant temperature stir 12 hours until formed evenly, water white transparency shape ionic liquid;
B. electrolyte solution preparation: joined by excessive Zinc oxide powder (analytical pure) in the ionic liquid that step a prepares, constant temperature stirs 10 hours at 60 DEG C ~ 100 DEG C, obtains the choline chloride/urea ionic liquid containing saturated zinc oxide;
C. the formation of cell system: using polytetrafluoroethylene beaker as electrolyzer, platinum disk electrode is to electrode; Be working electrode also i.e. negative electrode through plating metal matrixes such as polishing, acidic activated copper sheets; Silver electrode is that reference electrode forms electrolyzer, carries out galvanic deposit;
D. the galvanic deposit synthesis process of micro-nano zinc layers: use constant-temperature temperature-control instrument to carry out temperature control to the cell system formed in above-mentioned steps c and remain on 40 DEG C ~ 100 DEG C, then applying electromotive force at cell system is-1.40V ~-1.70V, and controlling electrodeposition time is 25 ~ 60 minutes; In the galvanic deposit synthesis process of micro-nano zinc layers, by any several the processing parameters in regulating and controlling temperature, electromotive force and time parameter effectively, realize the effective control to micro-nano zinc layers feature in deposition process;
E. the product through above-mentioned steps d galvanic deposit gained is taken out from electrolyzer, first clean with deionized water, more repeatedly clean with dehydrated alcohol, finally carry out oven drying at low temperature and obtain densification, uniform micro-nano zinc layers.
Principle of the present invention: the electromotive force accurately controlling working electrode by electrochemistry three-electrode system make the zinc oxide that dissolves in ionogen working electrode also namely negative electrode be reduced into metallic zinc, generate oxygen to electrode occurs oxygen evolution reaction.
Compared with prior art, the inventive method has following substantive distinguishing features and significant advantage:
1. the present invention adopts the choline chloride/urea ionic liquid of recoverable to be electrolyte solution, has wide electrochemical window and avoids liberation of hydrogen side reaction.Employing zinc oxide is raw material, and ingredient requirement is low, prepares metal zinc layers by the direct galvanic deposit of electrochemical method.In addition, by accurately controlling electrochemical process parameter, reaching the accurate control to the growth of the forming core of metal refining zinc layers and pattern, is a kind of green high-efficient controlledly synthesis novel process;
2. the choline chloride/urea ionic liquid prepared in the present invention belongs to the one of room temperature fused salt, and electrochemical reaction process carries out at low temperatures, effectively prevent the dependence of high temperature, strong acid and strong base, greatly simplify conventional process flow, reduce cost;
3. the present invention is simple to operate, process control, and efficiency is high, does not produce other side reactions, production of easily magnifying.Ionic liquid environmental protection, can recirculation use, with low cost, energy consumption is low, is conducive to realizing suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention one prepares the short route schematic diagram of micro-nano zinc layers by the inventive method.
Fig. 2 is the current density-time curve preparing micro-nano zinc layers process by the inventive method by embodiment one galvanic deposit.
Fig. 3 is the XRD figure of the micro-nano zinc layers utilizing the inventive method to prepare by embodiment one galvanic deposit.
Fig. 4 is the SEM figure of the micro-nano zinc layers utilizing the inventive method galvanic deposit under different electromotive force to prepare.
Fig. 5 is the SEM figure utilizing the inventive method micro-nano zinc layers of preparing of galvanic deposit at different temperatures.
Embodiment
Details are as follows for specific embodiments of the invention.
embodiment one
In the present embodiment, as shown in Figure 1, the electrochemical preparation process of micro-nano zinc coating, comprises the following steps schema:
1. first get 116.35g choline chloride 60 and 100g urea mixes in beaker, under 80 ° of C, constant temperature stirs 12 little
Generate up to even, water white transparency shape ionic liquid, in the ionic liquid of synthesis, get 50ml be placed in polytetrafluoroethylene beaker stand-by.
2. get 5g Zinc oxide powder and be placed in choline chloride/urea ionic liquid, at 60 DEG C, constant temperature stirs 10 hours, obtains
Containing the choline chloride/urea ionic liquid of saturated zinc oxide.Using polytetrafluoroethylene beaker as electrolyzer, platinum disk electrode is to electrode, be working electrode through polishing, acidic activated copper sheet (0.4cm × 0.5cm), silver electrode is reference electrode, and above-mentioned three electrodes is fixed on assembling in tetrafluoroethylene electrolyzer and forms electro-deposition system.
The temperature adopting electrochemical workstation, constant-temperature temperature-control instrument and electric mantle to regulate and control electrodeposition process working electrode potential and electrolyzer Inner electrolysis matter respectively carries out galvanic deposit.Electrodeposition temperature is 60 DEG C, and adopting three-electrode system to control working electrode potential is-1.40V voltage, completes experiment, obtain densification, uniform micro-nano zinc coating after reaction carries out 25 minutes.Because choline chloride/urea ionic liquid has higher solubleness to zinc oxide, and form complex compound in the process of dissolving, weaken the bonding force of zinc in zinc oxide and oxygen, facilitate the carrying out of electrodeposit reaction, improve reaction efficiency.Only there is deposition and the oxygen uptake reaction of metallic zinc in whole reaction system, choline chloride/urea ionic liquid decomposes, and ionogen is capable of circulation repeatedly to be used.Finally from electrolyzer, take out galvanic deposit product, clean with deionized water, more repeatedly clean with dehydrated alcohol, finally the clean product obtained is carried out oven drying at low temperature, namely obtain densification, uniform micro-nano zinc coating.As shown in Figure 2, the XRD of the coating zinc product of acquisition as shown in Figure 3 (wherein copper diffraction peak is because coating matrix is that copper sheet causes) for the current density-time curve of electrodeposition process.The SEM figure of the coating zinc product obtained as shown in Figure 4 (a).Can find out that the product that the present embodiment obtains is pure Zn thing phase from XRD analysis, demonstrate the present invention fully and utilize the success of choline chloride/urea ionic liquid to prepare micro-nano zinc layers from zinc oxide galvanic deposit.The present embodiment, by control temperature and the parameter such as electromotive force, time, realizes metallic zinc coating growth morphology, the isoparametric effective control of size, for producing the controlled synthesis novel method providing a kind of micro-nano zinc coating completely newly.
embodiment two
The present embodiment is substantially identical with embodiment one, and its difference is:
In the present embodiment, electrodeposition temperature is 60 DEG C, and adopting three-electrode system to control working electrode potential is-1.50V voltage, completes experiment, obtain densification, uniform micro-nano zinc coating after reaction carries out 25 minutes.The SEM figure of the zinc coating product obtained as shown in Figure 4 (b).
embodiment three
The present embodiment is substantially identical with above-described embodiment one, and its difference is:
In the present embodiment, electrodeposition temperature is 60 DEG C, and adopting three-electrode system to control working electrode potential is-1.60V voltage, completes experiment, obtain densification, uniform micro-nano zinc coating after reaction carries out 25 minutes.The SEM figure of the zinc coating product obtained as shown in Figure 4 (c).
embodiment four
The present embodiment is substantially identical with above-described embodiment one, and its difference is:
In the present embodiment, electrodeposition temperature is 60 DEG C, and adopting three-electrode system to control working electrode potential is-1.70V voltage, completes experiment, obtain densification, uniform micro-nano zinc coating after reaction carries out 25 minutes.The SEM figure of the zinc coating product obtained is as shown in Fig. 4 (d).
embodiment five
The present embodiment is substantially identical with above-described embodiment one, and its difference is:
In the present embodiment, electrodeposition temperature is 40 DEG C, and adopting three-electrode system to control working electrode potential is-1.60V voltage, completes experiment, obtain densification, uniform micro-nano zinc coating after reaction carries out 25 minutes.The SEM figure of the zinc coating product obtained is as shown in Fig. 5 (a).
embodiment six
The present embodiment is substantially identical with above-described embodiment one, and its difference is:
In the present embodiment, electrodeposition temperature is 80 DEG C, and adopting three-electrode system to control working electrode potential is-1.60V voltage, completes experiment, obtain densification, uniform micro-nano zinc coating after reaction carries out 25 minutes.The SEM figure of the zinc coating product obtained is as shown in Fig. 5 (c).
embodiment seven
The present embodiment is substantially identical with above-described embodiment one, and its difference is:
In the present embodiment, electrodeposition temperature is 100 DEG C, and adopting three-electrode system to control working electrode potential is-1.60V voltage, completes experiment, obtain densification, uniform micro-nano zinc coating after reaction carries out 25 minutes.The SEM figure of the zinc coating product obtained is as shown in Fig. 5 (d).
Claims (1)
1. prepared a method for micro-nano zinc layers under low temperature by the direct galvanic deposit of zinc oxide, it is characterized in that there are following steps:
A. the preparation of choline chloride/urea ionic liquid: with choline chloride 60 and urea for initial feed, 1:2 mixes in molar ratio, at 80 DEG C constant temperature stir 12 hours until formed evenly, water white transparency shape ionic liquid;
B. electrolyte solution preparation: joined by excessive Zinc oxide powder (analytical pure) in the ionic liquid that step a prepares, constant temperature stirs 10 hours at 60 DEG C ~ 100 DEG C, obtains the choline chloride/urea ionic liquid containing saturated zinc oxide;
C. the formation of cell system: using polytetrafluoroethylene beaker as electrolyzer, platinum disk electrode is to electrode; Be working electrode also i.e. negative electrode through plating metal matrixes such as polishing, acidic activated copper sheets, silver electrode is that reference electrode forms electrolyzer, carries out galvanic deposit;
D. the galvanic deposit synthesis process of micro-nano zinc layers: use constant-temperature temperature-control instrument to carry out temperature control to the cell system formed in above-mentioned steps c and remain on 40 DEG C ~ 100 DEG C, then applying electromotive force at cell system is-1.40V ~-1.70V, and controlling electrodeposition time is 25 ~ 60 minutes; In the galvanic deposit synthesis process of micro-nano zinc layers, by any several the processing parameters in regulating and controlling temperature, electromotive force and time parameter effectively, realize the effective control to micro-nano zinc layers feature in deposition process;
E. the product through above-mentioned steps d galvanic deposit gained is taken out from electrolyzer, first clean with deionized water, more repeatedly clean with dehydrated alcohol, finally carry out oven drying at low temperature and obtain densification, uniform micro-nano zinc layers.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106435659A (en) * | 2016-11-21 | 2017-02-22 | 江苏梦得新材料科技有限公司 | Electro-galvanizing brightening agent |
CN108546829A (en) * | 2018-04-09 | 2018-09-18 | 苏州大学 | A method of the processing of the synthetical recovery of metallurgical dust sludge containing zinc |
CN108642520A (en) * | 2018-06-28 | 2018-10-12 | 南京信息工程大学 | A method of zinc is generated based on choline chloride-malonic acid eutectic system |
CN108707934A (en) * | 2018-06-28 | 2018-10-26 | 南京信息工程大学 | A kind of method of fast-growth thickness spelter coating on Copper substrate |
CN108754556A (en) * | 2018-06-28 | 2018-11-06 | 南京信息工程大学 | A kind of method of simple system electrodepositing zinc coating |
CN110029370A (en) * | 2019-04-17 | 2019-07-19 | 上海大学 | By the method for low value cupro-nickel composite ore electro-deposition preparation high level ternary alloy three-partalloy |
CN110714212A (en) * | 2019-10-12 | 2020-01-21 | 常州大学 | Method for preparing super-hydrophobic nickel film in aqueous solution system by nickel chloride one-step method |
CN111261855A (en) * | 2020-01-20 | 2020-06-09 | 广东省材料与加工研究所 | Zinc composite electrode material, preparation method thereof and battery |
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CN102191517A (en) * | 2010-03-10 | 2011-09-21 | 中国科学院过程工程研究所 | Method of electroplating zinc, nickel, molybdenum and their alloys by using ionic liquid |
CN104562090A (en) * | 2014-12-30 | 2015-04-29 | 昆明理工大学 | Method for preparing nano-porous copper through in-situ electrolysis of eutectic ionic liquid |
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CN102191517A (en) * | 2010-03-10 | 2011-09-21 | 中国科学院过程工程研究所 | Method of electroplating zinc, nickel, molybdenum and their alloys by using ionic liquid |
CN104562090A (en) * | 2014-12-30 | 2015-04-29 | 昆明理工大学 | Method for preparing nano-porous copper through in-situ electrolysis of eutectic ionic liquid |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106435659A (en) * | 2016-11-21 | 2017-02-22 | 江苏梦得新材料科技有限公司 | Electro-galvanizing brightening agent |
CN108546829A (en) * | 2018-04-09 | 2018-09-18 | 苏州大学 | A method of the processing of the synthetical recovery of metallurgical dust sludge containing zinc |
CN108642520A (en) * | 2018-06-28 | 2018-10-12 | 南京信息工程大学 | A method of zinc is generated based on choline chloride-malonic acid eutectic system |
CN108707934A (en) * | 2018-06-28 | 2018-10-26 | 南京信息工程大学 | A kind of method of fast-growth thickness spelter coating on Copper substrate |
CN108754556A (en) * | 2018-06-28 | 2018-11-06 | 南京信息工程大学 | A kind of method of simple system electrodepositing zinc coating |
CN110029370A (en) * | 2019-04-17 | 2019-07-19 | 上海大学 | By the method for low value cupro-nickel composite ore electro-deposition preparation high level ternary alloy three-partalloy |
CN110714212A (en) * | 2019-10-12 | 2020-01-21 | 常州大学 | Method for preparing super-hydrophobic nickel film in aqueous solution system by nickel chloride one-step method |
CN111261855A (en) * | 2020-01-20 | 2020-06-09 | 广东省材料与加工研究所 | Zinc composite electrode material, preparation method thereof and battery |
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