CN102199783A - Nickel electroplating liquid, and preparation method for super-hydrophobic nickel plating layer using same - Google Patents
Nickel electroplating liquid, and preparation method for super-hydrophobic nickel plating layer using same Download PDFInfo
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- CN102199783A CN102199783A CN 201110152051 CN201110152051A CN102199783A CN 102199783 A CN102199783 A CN 102199783A CN 201110152051 CN201110152051 CN 201110152051 CN 201110152051 A CN201110152051 A CN 201110152051A CN 102199783 A CN102199783 A CN 102199783A
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- nickel
- nickel plating
- super
- hydrophobic
- plating solution
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 176
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 95
- 238000007747 plating Methods 0.000 title claims abstract description 53
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 28
- 238000009713 electroplating Methods 0.000 title abstract description 18
- 239000007788 liquid Substances 0.000 title abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 7
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims abstract description 29
- 235000019743 Choline chloride Nutrition 0.000 claims abstract description 29
- 229960003178 choline chloride Drugs 0.000 claims abstract description 29
- 239000002608 ionic liquid Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims description 41
- 238000000576 coating method Methods 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 38
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000003518 caustics Substances 0.000 abstract description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract 1
- 150000002815 nickel Chemical class 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000012467 final product Substances 0.000 description 6
- 229910000806 Latten Inorganic materials 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000004070 electrodeposition Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 231100001010 corrosive Toxicity 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a nickel electroplating liquid, and a preparation method for a super-hydrophobic nickel plating layer using the same. The nickel electroplating liquid is composed of a choline-chloride-based ionic liquid used as a solvent and NiCl2.6H2O or NiCl2 used as a solute, wherein the mol concentration of the solute is 0.1-3 mol/L. The preparation method for the super-hydrophobic nickel plating layer using the nickel electroplating liquid comprises the following step of electroplating in the nickel electroplating liquid with pure nickel as an anode and the workpiece to be electroplated as a cathode at the temperature of the nickel electroplating liquid from room temperature to 200 DEG C and electroplating voltage of 0.2-2 V. The nickel electroplating liquid provided by the invention has simple components, is convenient to prepare and is environmentally-friendly. The preparation method for the super-hydrophobic nickel plating layer using the nickel electroplating liquid has the advantages of simple and controllable process, no corrosive substances and no vapor discharge during the electroplating process, and is beneficial to mass production. More prominent characteristics are that the obtained nickel plating layer has super-hydrophobic property, a contact angle larger than 160 degrees and a sliding angle smaller than 2 degrees.
Description
Technical field
The invention belongs to metal plating prepared by electrodeposition field, be specifically related to a kind of nickel plating solution and use this nickel plating solution to prepare the method for super-hydrophobic nickel coating.
Background technology
Super-hydrophobic (hydrophobic) surface generally is meant and the contact angle of the water surfaces greater than 150 degree, and there is potential widely application in fields such as, hull drag reduction anticorrosion, anti-icing at material surface and microfluid.The pure metal surface generally shows as water-wet behavior, if make the metallic surface obtain superhydrophobic characteristic, adopt two-step approach to handle usually: at first roughened will be carried out in the metallic surface, and then carries out the covering of low surface energy material.The two-step process more complicated, time-consuming, and the super hydrophobic surface less stable that makes, the widespread use of super hydrophobic surface is brought difficulty.Studies show that in a large number material surface is carried out nanometer handles the hydrophobic property that can improve material greatly, and electro-deposition techniques is the effective means that realizes the metallic surface large-area nanoization.However, at present, also there is certain difficulty in the technology on the pure metal surface by single stage method galvanic deposit acquisition superhydrophobic characteristic; In addition, the electro-deposition techniques that adopts adopts the aqueous electrolysis liquid system more at present, owing to contain strong acid or highly basic in the electrolytic solution, therefore environment and operator is damaged.Therefore, the electro-deposition techniques of exploitation environmental protection realizes that the technology of the super-hydrophobic metallic surface of large-area preparation is significant.
Summary of the invention
The invention provides a kind of nickel plating solution and use this nickel plating solution to prepare the method for super-hydrophobic nickel coating, this nickel plating solution safety and environmental protection uses the electrodeposition technology simple controllable of this electroplate liquid, safety and environmental protection, and the nickel coating for preparing has superhydrophobic characteristic.
A kind of nickel plating solution, with choline chloride 60 base ionic liquid as solvent, with NiCl
26H
2O or NiCl
2Be solute; Wherein, the volumetric molar concentration of described solute is 0.1～3 mol, and described choline chloride 60 base ionic liquid is that mol ratio is that 1: 2 choline chloride 60 and ethylene glycol mixtures or mol ratio are that 1: 2 the choline chloride 60 and the mixed solution or the mol ratio of propylene glycol are 1: 2 the choline chloride 60 and the mixed solution of urea.
Each above-mentioned chemical is the conventional chemical product, can buy from market.Wherein the molecular formula of choline chloride 60 is C
5H
14ClNO, products C as code are 67-48-1.
Above-mentioned nickel plating solution can be prepared by following method:
With NiCl
26H
2O or NiCl
2Being dissolved in choline chloride 60 base ionic liquid in proportion gets final product.
A kind of method of using described nickel plating solution to prepare super-hydrophobic nickel coating, with the pure nickel is anode,, electroplates in described nickel plating solution as negative electrode with the electroplated workpiece, the temperature of described nickel plating solution is room temperature～200 ℃, and the voltage during plating is 0.2～2V.
The volumetric molar concentration of solute is the 0.5-1.5 mol in the preferred described nickel plating solution, super-hydrophobic the best of the nickel coating that obtains.
The temperature of preferred described nickel plating solution is 60～100 ℃, and the nickel coating quality of gained is good, is difficult for cracking.
The plating power supply can adopt the direct supply or the pulse power.After electroplate finishing, adopt the first alcohol and water to clean coating successively usually and dry up.
The thickness of the nickel coating that plating makes is determined by electroplating time.
Among the present invention, adopt choline chloride 60 base ionic liquid as the nickel plating solution solvent, because it is to be made of specific organic cation and negatively charged ion, in room temperature or near the molten salt system that is in a liquid state under the room temperature, thus the physical and chemical performance with a series of uniquenesses, as the dielectric solvent of electrochemical reaction, compare with water-based electroplate liquid or organic solvent, have unique advantage, as the reaction efficiency height, electrochemical window is wide, vapour pressure is extremely low, thermostability is high, and also environmentally friendly.
Compared with prior art, the present invention has following beneficial technical effects:
Nickel plating solution composition of the present invention is simple, and preparation is convenient, and is environmentally friendly.Use this nickel plating solution to prepare the technology simple controllable of nickel coating, do not contain corrosives, do not have discharge of steam in the electroplating process.The gained nickel coating has superhydrophobic characteristic, contact angle greater than 160 ° and roll angle less than 2 °.The super-hydrophobic nickel coating that the present invention makes can be applicable to the occasion that ships outside surface, metal pipe internal wall etc. need reduce water resistance.
Description of drawings
Fig. 1 is the scanning electron photomicrograph of the super-hydrophobic nickel coating of the inventive method preparation.
Embodiment
Describe the present invention in detail below in conjunction with embodiment, but the present invention is not limited to this.
Embodiment 1:
Choline chloride 60 ((Shanghai) Co., Ltd. buys from Aladdin reagent) and ethylene glycol 75 ℃ under are mixed according to mol ratio at 1: 2, obtain choline chloride 60 base ionic liquid.With 5 gram NiCl
26H
2O is dissolved in the 40ml choline chloride 60 base ionic liquid, promptly obtains nickel plating solution.
As anode, latten(-tin) is electroplated in the above-mentioned nickel plating solution that makes as negative electrode with electrolytic nickel, plating voltage is 1V, and the temperature of nickel plating solution is 90 ℃, electroplating time 1 hour, after electroplate finishing, with the first alcohol and water coating is cleaned successively and dries up and get final product.
The about 5 μ m of the above-mentioned nickel coating thickness that makes.Scanning electron photomicrograph shows that the nickel coating surface is made of the nickel thin slice of nanoscale, and its electron scanning micrograph as shown in Figure 1.
Further contact angle and roll angle measurement are carried out in this nickel coating surface.The contact angle testing method is for to be added drop-wise to 1 μ l water droplet on the nickel coating surface of being tested, angle by digital camera record water droplet and nickel coating surface point of contact place's water droplet profile and nickel coating surface, this angle illustrates that greater than 150 ° measured surface has superhydrophobic characteristic.Roll angle is measured and is adopted the nickel coating surface that tilts gradually, writes down water droplet when the generation of nickel coating surface is rolled, the angle of nickel coating surface and horizontal plane, and this angle is more little, illustrates that the performance of super hydrophobic surface is excellent more.Measuring result is: less than 2 °, as seen this nickel coating has superhydrophobic characteristic to contact angle greater than 160 ° and roll angle.
Embodiment 2:
Choline chloride 60 ((Shanghai) Co., Ltd. buys from Aladdin reagent) and propylene glycol 75 ℃ under are mixed according to mol ratio at 1: 2, obtain choline chloride 60 base ionic liquid.With 2.0 gram NiCl
2Be dissolved in the 40ml choline chloride 60 base ionic liquid, promptly obtain nickel plating solution.
With electrolytic nickel as anode, latten(-tin) is as negative electrode, in the above-mentioned nickel plating solution that makes, electroplate, carry out galvanic deposit in the pulsed deposition mode, plating voltage is 1V, the pulse-repetition no requirement (NR), the temperature of nickel plating solution is 60 ℃, electroplating time 1 hour after electroplate finishing, cleans successively and dries up coating with the first alcohol and water and get final product.
The about 2 μ m of the above-mentioned nickel coating thickness that makes.Contact angle and roll angle measurement discovery are carried out in this nickel coating surface, and contact angle is greater than 150 °, and roll angle is less than 2 °, and as seen this nickel coating has superhydrophobic characteristic.
Embodiment 3:
Choline chloride 60 ((Shanghai) Co., Ltd. buys from Aladdin reagent) and urea 75 ℃ under are mixed according to mol ratio at 1: 2, obtain choline chloride 60 base ionic liquid.With 13 gram NiCl
26H
2O is dissolved in the 40ml choline chloride 60 base ionic liquid, promptly obtains nickel plating solution.
With electrolytic nickel as anode, latten(-tin) is as negative electrode, in the above-mentioned nickel plating solution that makes, electroplate, carry out galvanic deposit with direct supply, plating voltage is 0.5V, the pulse-repetition no requirement (NR), the temperature of nickel plating solution is 100 ℃, electroplating time 1 hour after electroplate finishing, cleans successively and dries up coating with the first alcohol and water and get final product.
The about 12 μ m of the above-mentioned nickel coating thickness that makes.Contact angle and roll angle measurement discovery are carried out in this nickel coating surface, and contact angle is greater than 160 °, and roll angle is less than 2 °.As seen this nickel coating has superhydrophobic characteristic.
Embodiment 4:
Choline chloride 60 ((Shanghai) Co., Ltd. buys from Aladdin reagent) and ethylene glycol 75 ℃ under are mixed according to mol ratio at 1: 2, obtain choline chloride 60 base ionic liquid.With 10 gram NiCl
26H
2O is dissolved in the 40ml choline chloride 60 base ionic liquid, promptly obtains nickel plating solution.
As anode, latten(-tin) is electroplated in the above-mentioned nickel plating solution that makes as negative electrode with electrolytic nickel, plating voltage is 1.5V, and the temperature of nickel plating solution is 40 ℃, electroplating time 1 hour, after electroplate finishing, with the first alcohol and water coating is cleaned successively and dries up and get final product.
The about 6 μ m of the above-mentioned nickel coating thickness that makes.Contact angle and roll angle measurement discovery are carried out in this nickel coating surface, and contact angle is greater than 160 °, and roll angle is less than 5 °.As seen this nickel coating has superhydrophobic characteristic.
Embodiment 5:
Choline chloride 60 ((Shanghai) Co., Ltd. buys from Aladdin reagent) and ethylene glycol 75 ℃ under are mixed according to mol ratio at 1: 2, obtain choline chloride 60 base ionic liquid.With 20 gram NiCl
26H
2O is dissolved in the 40ml choline chloride 60 base ionic liquid, promptly obtains nickel plating solution.
As anode, latten(-tin) is electroplated in the above-mentioned nickel plating solution that makes as negative electrode with electrolytic nickel, plating voltage is 1V, and the temperature of nickel plating solution is 60 ℃, electroplating time 1 hour, after electroplate finishing, with the first alcohol and water coating is cleaned successively and dries up and get final product.
The about 15 μ m of the above-mentioned nickel coating thickness that makes.Contact angle and roll angle are carried out in this nickel coating surface measure and find contact angle greater than 150 °, roll angle is less than 5 °.As seen this nickel coating has superhydrophobic characteristic.
Claims (4)
1. a nickel plating solution is characterized in that, with choline chloride 60 base ionic liquid as solvent, with NiCl
26H
2O or NiCl
2Be solute; Wherein, the volumetric molar concentration of described solute is 0.1～3 mol, and described choline chloride 60 base ionic liquid is that mol ratio is that 1: 2 choline chloride 60 and ethylene glycol mixtures or mol ratio are that 1: 2 the choline chloride 60 and the mixed solution or the mol ratio of propylene glycol are 1: 2 the choline chloride 60 and the mixed solution of urea.
2. use nickel plating solution as claimed in claim 1 to prepare the method for super-hydrophobic nickel coating, it is characterized in that, with the pure nickel is anode, with the electroplated workpiece as negative electrode, in described nickel plating solution, electroplate, the temperature of described nickel plating solution is room temperature～200 ℃, and the voltage during plating is 0.2～2V.
3. method as claimed in claim 2 is characterized in that, in the described nickel plating solution, the volumetric molar concentration of described solute is 0.5～1.5 mol.
4. method as claimed in claim 2 is characterized in that, the temperature of described nickel plating solution is 60～100 ℃.
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|---|---|---|---|
| CN 201110152051 CN102199783A (en) | 2011-06-08 | 2011-06-08 | Nickel electroplating liquid, and preparation method for super-hydrophobic nickel plating layer using same |
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|---|---|---|---|
| CN 201110152051 CN102199783A (en) | 2011-06-08 | 2011-06-08 | Nickel electroplating liquid, and preparation method for super-hydrophobic nickel plating layer using same |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677132A (en) * | 2012-05-28 | 2012-09-19 | 大连理工大学 | Method for preparing super-hydrophobic coating of metallic matrix |
| CN103382564A (en) * | 2013-07-18 | 2013-11-06 | 华南理工大学 | Super-hydrophobic cobalt plating of metal surface and preparation method for super-hydrophobic cobalt plating |
| CN104005066A (en) * | 2014-05-16 | 2014-08-27 | 华南理工大学 | Magnesium alloy surface super hydrophobic membrane layer and preparation method and application thereof |
| CN104313655A (en) * | 2014-10-16 | 2015-01-28 | 昆明理工大学 | Method for electroplating Ni-Fe alloy with ionic liquid |
| CN105293427A (en) * | 2015-09-21 | 2016-02-03 | 南开大学 | Preparation method of super-hydrophobic surface based on limited local plating of meniscus |
| CN106435672A (en) * | 2016-08-26 | 2017-02-22 | 无锡光旭新材料科技有限公司 | Tin, zinc and nickel electroplating method based on choline chloride-malic acid deep-eutectic solvents |
| RU2623514C2 (en) * | 2015-01-12 | 2017-06-27 | Федеральное государственное автономное образовательное учреждение высшего образования "Волгоградский государственный университет" | Electrolyte for galvanic sedimentation of nickel-aluminium coatings |
| WO2018058457A1 (en) * | 2016-09-29 | 2018-04-05 | 东北石油大学 | Method and device for preparing high-durability super-hydrophobic film on inner wall of slender metal pipe |
| CN108085723A (en) * | 2017-11-28 | 2018-05-29 | 昆明理工大学 | A kind of method of eutectic solvent Nickel-Chromium Electrodeposit coating |
| CN108823617A (en) * | 2018-06-25 | 2018-11-16 | 宁波中材钰翔新材料科技有限公司 | A kind of preparation method of super water repellent metal mesh |
| CN110205658A (en) * | 2019-07-16 | 2019-09-06 | 南昌航空大学 | A kind of process of the porous nickel coating of the electro-deposition from ionic liquid at room temperature |
| 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 |
| CN113174617A (en) * | 2021-04-29 | 2021-07-27 | 常州大学 | Method for preparing super-hydrophobic Zn-Fe alloy coating in eutectic ionic liquid through electrodeposition |
| CN114959818A (en) * | 2022-05-30 | 2022-08-30 | 阜阳师范大学 | Method for preparing super-hydrophobic coating by one-step electrodeposition in eutectic solvent |
| CN114959817A (en) * | 2022-05-27 | 2022-08-30 | 山东科技大学 | Super-hydrophobic Ni-CeO on surface of pipeline steel 2 Method for producing a layer and use thereof |
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| CN102677132A (en) * | 2012-05-28 | 2012-09-19 | 大连理工大学 | Method for preparing super-hydrophobic coating of metallic matrix |
| CN103382564A (en) * | 2013-07-18 | 2013-11-06 | 华南理工大学 | Super-hydrophobic cobalt plating of metal surface and preparation method for super-hydrophobic cobalt plating |
| CN103382564B (en) * | 2013-07-18 | 2016-10-05 | 华南理工大学 | Metal surface superhydrophobic cobalt coating and preparation method thereof |
| CN104005066A (en) * | 2014-05-16 | 2014-08-27 | 华南理工大学 | Magnesium alloy surface super hydrophobic membrane layer and preparation method and application thereof |
| CN104313655A (en) * | 2014-10-16 | 2015-01-28 | 昆明理工大学 | Method for electroplating Ni-Fe alloy with ionic liquid |
| RU2623514C2 (en) * | 2015-01-12 | 2017-06-27 | Федеральное государственное автономное образовательное учреждение высшего образования "Волгоградский государственный университет" | Electrolyte for galvanic sedimentation of nickel-aluminium coatings |
| CN105293427A (en) * | 2015-09-21 | 2016-02-03 | 南开大学 | Preparation method of super-hydrophobic surface based on limited local plating of meniscus |
| CN106435672A (en) * | 2016-08-26 | 2017-02-22 | 无锡光旭新材料科技有限公司 | Tin, zinc and nickel electroplating method based on choline chloride-malic acid deep-eutectic solvents |
| WO2018058457A1 (en) * | 2016-09-29 | 2018-04-05 | 东北石油大学 | Method and device for preparing high-durability super-hydrophobic film on inner wall of slender metal pipe |
| US11078572B2 (en) | 2016-09-29 | 2021-08-03 | Northeast Petroleum University | Method and device for preparing high strength and durable super-hydrophobic film layer on inner wall of elongated metal tube |
| CN108085723A (en) * | 2017-11-28 | 2018-05-29 | 昆明理工大学 | A kind of method of eutectic solvent Nickel-Chromium Electrodeposit coating |
| CN108823617A (en) * | 2018-06-25 | 2018-11-16 | 宁波中材钰翔新材料科技有限公司 | A kind of preparation method of super water repellent metal mesh |
| CN110205658A (en) * | 2019-07-16 | 2019-09-06 | 南昌航空大学 | A kind of process of the porous nickel coating of the electro-deposition from ionic liquid at room temperature |
| 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 |
| CN113174617A (en) * | 2021-04-29 | 2021-07-27 | 常州大学 | Method for preparing super-hydrophobic Zn-Fe alloy coating in eutectic ionic liquid through electrodeposition |
| CN114959817A (en) * | 2022-05-27 | 2022-08-30 | 山东科技大学 | Super-hydrophobic Ni-CeO on surface of pipeline steel 2 Method for producing a layer and use thereof |
| CN114959818A (en) * | 2022-05-30 | 2022-08-30 | 阜阳师范大学 | Method for preparing super-hydrophobic coating by one-step electrodeposition in eutectic solvent |
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Application publication date: 20110928 |