CN110205658A - A kind of process of the porous nickel coating of the electro-deposition from ionic liquid at room temperature - Google Patents

A kind of process of the porous nickel coating of the electro-deposition from ionic liquid at room temperature Download PDF

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Publication number
CN110205658A
CN110205658A CN201910640455.2A CN201910640455A CN110205658A CN 110205658 A CN110205658 A CN 110205658A CN 201910640455 A CN201910640455 A CN 201910640455A CN 110205658 A CN110205658 A CN 110205658A
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porous nickel
electro
deposition
room temperature
ionic liquid
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CN110205658B (en
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田礼煕
傅伟海
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Nanchang Hangkong University
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Nanchang Hangkong University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces

Abstract

The process of the invention discloses a kind of from the ionic liquid at room temperature porous nickel coating of electro-deposition, comprising the following steps: 1) mix choline chloride with ethylene glycol, and heating stirring to hamming is clarified;2) CrCl is added3·6H2O and NiCl2·6H2O continues to stir to transparent;3) additive NaF is added to continue to stir;4) it is electroplated using the metal base for needing to cover porous nickel sheet as cathode, anode is insoluble anode;5) plating piece is cleaned with cleaning solution and dry.The present invention passes through additive NaF and a certain amount of CrCl3·6H2The effect of O, the forming core and growth course for changing nickel, directly grow the nickel coating of porous form, compare existing porous nickel technique for preparing coating, it is efficiently convenient without additional subsidiary conditions (such as bubble hydrogen auxiliary law) or to the postprocessing working procedures (such as removal alloying method) of coating.

Description

A kind of process of the porous nickel coating of the electro-deposition from ionic liquid at room temperature
Technical field
The present invention relates to a kind of electroplating technologies, and in particular to a kind of porous nickel coating of the electro-deposition from ionic liquid at room temperature Process.
Background technique
Nickel is a kind of nearly silvery white non-ferrous metal, has ferromagnetism and good ductility, atomic weight 58.71, density is 8.9 g/cm3, 1453 DEG C of fusing point.
Traditional nickel coating is generally used for incrustation and anticorrosion field, porous nickel coating be then applied to electrode, catalysis, The fields such as sensing, heat exchange.
Plating porous nickel sheet mainly has bubble hydrogen auxiliary law and removal alloying method at present, and the formation needs of porous nickel coating are borrowed It helps auxiliary process or coating is post-processed, technique is relatively cumbersome.
Summary of the invention
For the above-mentioned prior art, the technical problem to be solved in the present invention is that providing, a kind of technological operation is simple, deposits High-efficient, the regulatable porous nickel coating of the electro-deposition from ionic liquid at room temperature of coating average pore size process.
In order to solve the above technical problems, the present invention provides a kind of from the ionic liquid at room temperature porous nickel coating of electro-deposition Process, specifically includes the following steps:
(1) choline chloride is mixed with ethylene glycol, and heating stirring is to transparent clarification;
(2) CrCl is added3·6H2O and NiCl2·6H2O continues to stir to transparent;
(3) additive NaF is added to continue to stir;
(4) it is electroplated using the metal base for needing to cover porous nickel sheet as cathode, anode is insoluble anode;
(5) plating piece is cleaned with cleaning solution and dry.
More preferably, in the step (1), the mass ratio of choline chloride and ethylene glycol is 1:2 ~ 1:3, and heating temperature is 80 DEG C ~85 DEG C.
More preferably, in the step (2), the molar ratio of Cr and Ni are that the sum of molar concentration of 0.5~1, Cr and Ni is not high In 1.5 mol/L.
More preferably, in the step (3), the additive amount of NaF is 0.1mol/L~0.8mol/L.
More preferably, in the step (4), current density 0.3A/dm2~0.6A/dm2, temperature is 50 DEG C~65 DEG C, electricity Plate time >=15 min.
More preferably, in the step (4), anode is platinum plate electrode or titanium platinized electrode.
More preferably, in the step (5), cleaning solution is organic solvent.
Compared with prior art, the beneficial effects of the present invention are: passing through additive NaF and a certain amount of CrCl3·6H2The work of O With, while cooperating lower current density, and it can change the forming core and growth course of nickel in this way, it is more so as to directly grow The nickel coating of pore morphology is not necessarily to additional subsidiary conditions (such as bubble hydrogen auxiliary law) compared to the preparation process of existing porous nickel coating Or (such as removal alloying method) is post-processed to coating, it is efficiently convenient.
Detailed description of the invention
Fig. 1 is the microscopic appearance of the porous nickel coating that obtains under a scanning electron microscope in the embodiment of the present invention 1;
Fig. 2 is the microscopic appearance of the porous nickel coating that obtains under a scanning electron microscope in the embodiment of the present invention 2;
Fig. 3 is the microscopic appearance of the porous nickel coating that obtains under a scanning electron microscope in the embodiment of the present invention 3.
Specific embodiment
The present invention is further described with preferred embodiment with reference to the accompanying drawing.
Embodiment 1:
The process of the present invention provides a kind of from the ionic liquid at room temperature porous nickel coating of electro-deposition, specific process step is such as Under:
1, it weighs 100g choline chloride and 300g ethylene glycol is placed in a beaker, with 80 DEG C of 6 h of heating stirring in oil bath pan, obtain Transparent supernatant liquid;
2,33gCrCl is weighed3·6H2O and 30gNiCl2·6H2O is added in beaker and continues to stir 1h, obtains transparent green liquid Body;
3,4 g NaF are added, continue to stir 30 min;
4, the nickel sheet for cutting certain size is electroplated using nickel sheet as cathode by anode of titanium platinized electrode, and current density is 0.3 A/dm2, temperature is 65 DEG C, and electroplating time is 30 min;
5, the nickel sheet after plating is soaked in acetic acid, 15min is cleaned in supersonic wave cleaning machine, in air dry oven after taking-up In with 60 DEG C of dry 10min, obtain nickel plating piece.
The surface microscopic topographic of the porous nickel coating as shown in Figure 1 obtained for the present embodiment under a scanning electron microscope, Its coating shows apparent porous form, and pore size is about 1 μm ~ 2 μm, and global tissue structure is relatively uniform.
Embodiment 2:
The processing step of the porous nickel coating of the present embodiment electro-deposition from ionic liquid at room temperature is as follows:
1, it weighs 100g choline chloride and 300g ethylene glycol is placed in a beaker, with 80 DEG C of 6 h of heating stirring in oil bath pan, obtain Transparent supernatant liquid;
2,33gCrCl is weighed3·6H2O and 30gNiCl2·6H2O is added in beaker and continues to stir 1h, obtains transparent green liquid Body;
3,4 g NaF are added, continue to stir 30 min;
4, the nickel sheet for cutting certain size is electroplated using nickel sheet as cathode by anode of titanium platinized electrode, and current density is 0.5 A/dm2, temperature is 65 DEG C, and electroplating time is 30 min;
5, the nickel sheet after plating is soaked in acetic acid, 15min is cleaned in supersonic wave cleaning machine, in air dry oven after taking-up In with 60 DEG C of dry 10 min, obtain nickel plating piece.
It is illustrated in figure 2 the surface microscopic topographic of porous nickel coating that the present embodiment obtains under a scanning electron microscope, Compared to embodiment 1, with the increase of current density, increase tendency is presented in coating aperture, and pore size is about 3 μm ~ 5 μ m。
Embodiment 3:
The processing step of the porous nickel coating of the present embodiment electro-deposition from ionic liquid at room temperature is as follows:
1, it weighs 100g choline chloride and 300g ethylene glycol is placed in a beaker, with 80 DEG C of heating stirring 6h in oil bath pan, obtain Transparent supernatant liquid;
2,33gCrCl is weighed3·6H2O and 30gNiCl2·6H2O is added in beaker and continues to stir 1h, obtains transparent green liquid Body;
3,6g NaF is added, continues to stir 30 min;
4, the nickel sheet for cutting certain size is electroplated using nickel sheet as cathode by anode of titanium platinized electrode, and current density is 0.6 A/dm2, temperature is 65 DEG C, and electroplating time is 30 min;
5, the nickel sheet after plating is soaked in acetic acid, 15 min is cleaned in supersonic wave cleaning machine, in forced air drying after taking-up 60 DEG C of 10 min of drying in case obtain nickel plating piece.
It is illustrated in figure 3 the surface microscopic topographic of porous nickel coating that the present embodiment obtains under a scanning electron microscope, Compared to embodiment 1 and embodiment 2, when current density is higher and NaF additive amount is larger, coating aperture is in significantly increasing and not The regular increased trend of degree, and coating at this time is more loose, if continuing to increase current density on this basis, it will make The porous form of coating is by destruction until plating can not be gone up.
The above only expresses the preferred embodiment of the present invention, and the description thereof is more specific and detailed, but can not be because This and be interpreted as limitations on the scope of the patent of the present invention.It should be pointed out that for those of ordinary skill in the art, Under the premise of not departing from present inventive concept, several deformations can also be made, improves and substitutes, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (7)

1. a kind of process of the porous nickel coating of the electro-deposition from ionic liquid at room temperature, which comprises the following steps:
(1) choline chloride is mixed with ethylene glycol, and heating stirring to hamming is clarified;
(2) CrCl is added3·6H2O and NiCl2· 6H2O continues to stir to transparent;
(3) additive NaF is added to continue to stir;
(4) it is electroplated using the metal base for needing to cover porous nickel sheet as cathode, anode is insoluble anode;
(5) plating piece is cleaned with cleaning solution and dry.
2. a kind of process of porous nickel coating of the electro-deposition from ionic liquid at room temperature according to claim 1, special Sign is: in the step (1), the mass ratio of choline chloride and ethylene glycol is 1:2 ~ 1:3, and heating temperature is 80 DEG C~85 DEG C.
3. a kind of process of porous nickel coating of the electro-deposition from ionic liquid at room temperature according to claim 1, special Sign is: in the step (2), the molar ratio of Cr and Ni are that the sum of molar concentration of 0.5~3, Cr and Ni is not higher than 1.5 mol/L。
4. a kind of process of porous nickel coating of the electro-deposition from ionic liquid at room temperature according to claim 1, special Sign is: in the step (3), the additive amount of NaF is the mol/L of 0.1 mol/L~0.8.
5. a kind of process of porous nickel coating of the electro-deposition from ionic liquid at room temperature according to claim 1, special Sign is: in the step (4), current density is 0.3 A/dm2~0.6 A/dm2, temperature is 50 DEG C~65 DEG C, electroplating time ≥15 min。
6. a kind of process of porous nickel coating of the electro-deposition from ionic liquid at room temperature according to claim 1, special Sign is: in the step (4), anode is platinum plate electrode or titanium platinized electrode.
7. a kind of process of porous nickel coating of the electro-deposition from ionic liquid at room temperature according to claim 1, special Sign is: in the step (5), cleaning solution is organic solvent.
CN201910640455.2A 2019-07-16 2019-07-16 Process method for electrodepositing porous nickel coating from room-temperature ionic liquid Active CN110205658B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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CN102199783A (en) * 2011-06-08 2011-09-28 浙江大学 Nickel electroplating liquid, and preparation method for super-hydrophobic nickel plating layer using same
CN102912391A (en) * 2012-10-12 2013-02-06 彩虹集团公司 Method for conducting low temperature electric deposition on nickel by utilizing ion liquid
CN106222693A (en) * 2016-08-23 2016-12-14 昆明理工大学 A kind of method that eutectic type ionic liquid prepares three-D nano-porous nickel
CN107335450A (en) * 2017-05-26 2017-11-10 昆明理工大学 A kind of method that electro-deposition prepares high catalysis analysis oxygen performance nanoporous ferronickel sulphur alloy in eutectic type ionic liquid
CN108220991A (en) * 2018-01-11 2018-06-29 昆明理工大学 A kind of method of the porous cobalt selenides of electrodeposited nanocrystalline in eutectic type ionic liquid

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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