CN104928732A - Nickel tungsten single-walled carbon nanotube composite plating solution, coating film and preparation method thereof - Google Patents

Nickel tungsten single-walled carbon nanotube composite plating solution, coating film and preparation method thereof Download PDF

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Publication number
CN104928732A
CN104928732A CN201510243164.1A CN201510243164A CN104928732A CN 104928732 A CN104928732 A CN 104928732A CN 201510243164 A CN201510243164 A CN 201510243164A CN 104928732 A CN104928732 A CN 104928732A
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China
Prior art keywords
carbon nanotube
walled carbon
nickel tungsten
nanotube composite
coating film
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CN201510243164.1A
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Chinese (zh)
Inventor
王军
傅敬强
唐荣武
万义秀
张小兵
曾云东
何毅
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Chongqing Natural Gas Purification Plant Southwest Oil And Gas Field Branch Of China National Petroleum Corp
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Chongqing Natural Gas Purification Plant Southwest Oil And Gas Field Branch Of China National Petroleum Corp
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Priority to CN201510243164.1A priority Critical patent/CN104928732A/en
Publication of CN104928732A publication Critical patent/CN104928732A/en
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Abstract

The invention discloses nickel tungsten single-walled carbon nanotube composite plating solution, a coating film and a preparation method thereof. SWCNTs having excellent mechanical performance and capable of effectively dispersing are leaded into the plating solution, and are effectively deposited and dispersed in a Ni-W matrix in the electroplating process. A Ni-W-SWCNTs composite coating film is successfully prepared on a carbon steel matrix through a pulse electroplating codeposition method. Nanotubes are dispersed in the Ni-W matrix; and as the competitive relation between crystal nucleation and growth is effectively changed in the codeposition process, and the coating film structure is improved, a deposited film layer becomes more uniform and compact, the intergranular corrosion is weakened, the dispersion path of a corrosion medium is lengthened, the self-corrosion potential is increased, the local corrosion is effectively inhibited, the stability of a passivated film is improved, and the corrosion resistance of the composite coating film is improved.

Description

A kind of nickel tungsten Single Walled Carbon Nanotube composite plating bath, plated film and preparation method thereof
Technical field
The present invention relates to electroplating technology field, particularly relate to a kind of nickel tungsten Single Walled Carbon Nanotube composite plating bath, plated film and preparation method thereof.
Background technology
The method of the current Ni-W of preparation plated film is mainly traditional Ni-W plated film electroplating technology, main plating solution composition and processing parameter as shown in table 1:
Table 1
Ni-W plated film preparation flow is: sand papering → ultrasonic cleaning → oil removing → ultrasonic cleaning → acid-wash activation → pulse plating → cleaning → aftertreatment → finished product.
Traditional electroplating technology is when preparing Ni-W plated film, current efficiency is low, liberation of hydrogen is serious, and electrochemical activity site is few, thus to cause in deposition process form that the residualinternal stress of plated film is large, crystallographic grain is thick, crystal boundary is obvious, coated surface dew point and the defect such as tiny crack is many.These defects can primarily induce serious local corrosion to occur in the practical application of Ni-W plated film, affect the mechanical property of rete, thus reduce the work-ing life of Ni-W plated film.
By introducing the Single Walled Carbon Nanotube that can effectively disperse in the plating solution, being amassed by its sorption-coprecipitation with NiW complex compound, reaching control crystalline structure thus improving the object of coated surface pattern.SWCNTs has larger specific surface area, and in deposition process, metal complex can be adsorbed in SWCNTs surface, and the formation for crystal provides more avtive spot, facilitates the formation of nucleus.On the other hand, SWCNTs can shield again the continued growth compared with macrocrystal, serves the effect slowing down crystal growth.In addition, the SWCNTs dispersed filler having a high strength is by dispersion-strengthened action in plated film, and the internal stress effectively decreasing plated film improves the mechanical property of plated film.Final Ni-W-SWCNTs composite film coating shows as that crystal grain is tiny, even structure is fine and close.Machinery and the solidity to corrosion of composite film coating all effectively improve.
Summary of the invention
The invention provides a kind of nickel tungsten Single Walled Carbon Nanotube composite plating bath, plated film and preparation method thereof.
The present invention adopts following technical scheme:
Nickel tungsten Single Walled Carbon Nanotube composite plating bath of the present invention consists of the following composition:
Preferred: plating solution of the present invention consists of the following composition:
Composite plating bath of the present invention is utilized to prepare the method for nickel tungsten Single Walled Carbon Nanotube composite film coating as follows:
First steel disc is utilized sand papering, then carry out ultrasonic cleaning, oil removing, again carry out ultrasonic cleaning, then carry out acid-wash activation, then carry out pulse plating, electroplated and cleaned, after aftertreatment, obtained finished product; Processing parameter in pulse plating process is: current density is 0.1-10A/dm 2, pH value is 6-9, and the time is 0.5-3h, and temperature is 50-80 DEG C, and power is 500-1500HZ, and dutycycle is 0.1-1.0.
The present invention compared with prior art, has following notable feature and beneficial effect:
The present invention introduces in the plating solution has good mechanical properties and the SWCNTs that can effectively disperse, and effectively SWCNTs deposition is scattered in Ni-W matrix in electroplating process.
Utilize composite plating bath of the present invention to prepare the method technique of nickel tungsten Single Walled Carbon Nanotube composite film coating simply, a small amount of SWCNTs effectively can improve the properties improving Ni-W plated film.
Successfully on plain steel, Ni-W-SWCNTs composite film coating has been prepared by the method for pulse plating codeposition.Nanotube dispersion is in Ni-W matrix, by the competitive relation changing crystal nucleation and growth effective in codeposition process, improve coating structure, make depositional coating become more even, fine and close, weaken intergranular corrosion, extend the evolving path of corrosive medium, improve corrosion potential, effectively inhibit local corrosion, improve the stability of passive film, thus improve the solidity to corrosion of composite film coating.
Embodiment
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field must belong to protection scope of the present invention according to the nonessential improvement more made for the present invention of the invention described above content and adjustment.
Embodiment 1
Nickel tungsten Single Walled Carbon Nanotube composite plating bath of the present invention consists of the following composition:
Composite plating bath of the present invention is utilized to prepare the method for nickel tungsten graphene oxide composite film coating as follows:
Composite plating bath of the present invention is utilized to prepare the method for nickel tungsten Single Walled Carbon Nanotube composite film coating as follows:
First steel disc is utilized sand papering, then carry out ultrasonic cleaning, oil removing, again carry out ultrasonic cleaning, then carry out acid-wash activation, then carry out pulse plating, electroplated and cleaned, after aftertreatment, obtained finished product; Processing parameter in pulse plating process is: current density is 0.1A/dm 2, pH value is 9, and the time is 0.5h, and temperature is 80 DEG C, and power is 500HZ, and dutycycle is 1.0.
Embodiment 2
Nickel tungsten Single Walled Carbon Nanotube composite plating bath of the present invention consists of the following composition:
Composite plating bath of the present invention is utilized to prepare the method for nickel tungsten Single Walled Carbon Nanotube composite film coating as follows:
First steel disc is utilized sand papering, then carry out ultrasonic cleaning, oil removing, again carry out ultrasonic cleaning, then carry out acid-wash activation, then carry out pulse plating, electroplated and cleaned, after aftertreatment, obtained finished product; Processing parameter in pulse plating process is: current density is 10A/dm 2, pH value is 6, and the time is 3h, and temperature is 50 DEG C, and power is 1500HZ, and dutycycle is 0.1.
Embodiment 3
Nickel tungsten Single Walled Carbon Nanotube composite plating bath of the present invention consists of the following composition:
Composite plating bath of the present invention is utilized to prepare the method for nickel tungsten Single Walled Carbon Nanotube composite film coating as follows:
First steel disc is utilized sand papering, then carry out ultrasonic cleaning, oil removing, again carry out ultrasonic cleaning, then carry out acid-wash activation, then carry out pulse plating, electroplated and cleaned, after aftertreatment, obtained finished product; Processing parameter in pulse plating process is: current density is 5A/dm 2, pH value is 8, and the time is 2h, and temperature is 70 DEG C, and power is 1000HZ, and dutycycle is 0.5.
Following Performance Detection is carried out to composite film coating prepared by the embodiment of the present invention 3:
JSM-7500F type scanning electronic microscope (SEM) is adopted to observe the surface topography of plated film.
By the elementary composition and content of INCA energy spectrometer (EDS) analytical test composite film coating.Ni constituent content is: 55-60wt.%, and content of element W is: 30-40wt.%, SWCNTs content is: 0-10wt.%
Adopt XPert PRO MPD type X-ray diffractometer (XRD), with Cu K α radiation, sweep limit is 10-80, researchs and analyses crystalline structure and the grain-size of composite film coating.Crystalline size is: 8-15nm.
By using CorrTest 310 type electrochemical workstation institute system for the solidity to corrosion of plated film.Use three-electrode system, wherein working electrode is No. 45 carbon steels depositing Ni-W-SWCNTs composite film coating, and useful area is 25mm × 15mm, and supporting electrode is platinum electrode, reference electrode is saturated calomel electrode (SCE), and corrosive medium is the NaCl aqueous solution of massfraction 3.5%.The impedance of composite film coating significantly improves, and corrosion potential rises to-0.30V from-0.50V, and corrosion electric current density is from 8.0uA/cm 2be down to 1.0uA/cm 2.
By the coefficient of sliding friction of MS-T3000 spin friction instrument test compound plated film, aluminum oxide abrading-ball, load 10N, rotating speed 300r/min, the test duration is 30min.The frictional coefficient of composite film coating reduces to 0.20 from 0.45.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.

Claims (4)

1. a nickel tungsten Single Walled Carbon Nanotube composite plating bath, is characterized in that: described plating solution consists of the following composition:
2. nickel tungsten Single Walled Carbon Nanotube composite plating bath as claimed in claim 1, is characterized in that: described plating solution consists of the following composition:
3. the nickel tungsten Single Walled Carbon Nanotube composite film coating electroplated by the composite plating bath described in claim 1 or 2.
4. nickel tungsten Single Walled Carbon Nanotube composite film coating as claimed in claim 3, is characterized in that: the preparation method of described nickel tungsten Single Walled Carbon Nanotube composite film coating is as follows:
First steel disc is utilized sand papering, then carry out ultrasonic cleaning, oil removing, again carry out ultrasonic cleaning, then carry out acid-wash activation, then carry out pulse plating, electroplated and cleaned, after aftertreatment, obtained finished product; Processing parameter in pulse plating process is: current density is 0.1-10A/dm 2, pH value is 6-9, and the time is 0.5-3h, and temperature is 50-80 DEG C, and power is 500-1500HZ, and dutycycle is 0.1-1.0.
CN201510243164.1A 2015-05-13 2015-05-13 Nickel tungsten single-walled carbon nanotube composite plating solution, coating film and preparation method thereof Pending CN104928732A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1721579A (en) * 2005-06-01 2006-01-18 上海工程技术大学 Method for preparing stable and dispersed composite plating solution used for carbon nanotube electro brush plating
CN102650072A (en) * 2011-02-24 2012-08-29 新光电气工业株式会社 Composite plating liquid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1721579A (en) * 2005-06-01 2006-01-18 上海工程技术大学 Method for preparing stable and dispersed composite plating solution used for carbon nanotube electro brush plating
CN102650072A (en) * 2011-02-24 2012-08-29 新光电气工业株式会社 Composite plating liquid

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
M. ALIOFKHAZRAEI ET AL: "Effect of the duty cycle of pulsed current on nanocomposite layers formed by pulsed electrodeposition", 《RARE METALS》 *
YI FAN ET AL: "Pulse Current Electrodeposition and Characterization of Ni-W-MWCNTs Nanocomposite Coatings", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 *
龚睿: "电沉积制备Ni-W非晶态合金镀层及其性能的研究", 《万方数据库 《华中科技大学硕士学位论文》》 *

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