CN112011817A - Ni-WS2Method for producing a coating - Google Patents
Ni-WS2Method for producing a coating Download PDFInfo
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- CN112011817A CN112011817A CN202010915107.4A CN202010915107A CN112011817A CN 112011817 A CN112011817 A CN 112011817A CN 202010915107 A CN202010915107 A CN 202010915107A CN 112011817 A CN112011817 A CN 112011817A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 239000010959 steel Substances 0.000 claims abstract description 99
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 89
- 238000009713 electroplating Methods 0.000 claims abstract description 38
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims abstract description 35
- 238000007747 plating Methods 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 239000002105 nanoparticle Substances 0.000 claims abstract description 20
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 17
- 238000005498 polishing Methods 0.000 claims abstract description 15
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000008021 deposition Effects 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004327 boric acid Substances 0.000 claims abstract description 9
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 9
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 9
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940081974 saccharin Drugs 0.000 claims abstract description 9
- 235000019204 saccharin Nutrition 0.000 claims abstract description 9
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims abstract description 9
- 239000000080 wetting agent Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 239000004519 grease Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 abstract description 33
- 230000007797 corrosion Effects 0.000 abstract description 32
- 238000000034 method Methods 0.000 abstract description 5
- 239000011241 protective layer Substances 0.000 abstract description 4
- 238000005282 brightening Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 13
- 238000002791 soaking Methods 0.000 description 9
- 238000012876 topography Methods 0.000 description 7
- 230000010287 polarization Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 3
- 240000002853 Nelumbo nucifera Species 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003075 superhydrophobic effect Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a Ni-WS2A method of preparing a coating comprising: grinding, polishing, cleaning and drying the X100 pipeline steel to obtain an X100 matrix; mixing deionized water, nickel sulfate, nickel chloride and boric acid, adjusting the pH value of the mixed solution to 3.3-3.7, and adding cetyl trimethyl ammonium bromide, saccharin, tungsten disulfide nanoparticles, a brightening agent and a wetting agent to obtain an electroplating solution; electroplating deposition is carried out in electroplating solution with pure nickel sheet as anode and X100 matrix as cathode, and current density is 4A/dm2The electroplating deposition time is 30-40 minutes, so that Ni-WS is prepared on the surface of the X100 pipeline steel2And (7) plating. The invention can prepare the protective layer with excellent corrosion resistance on the surface of the X100 pipeline steel, not only greatly enhances the corrosion resistance and the durability of the X100 pipeline steel, but also has simple preparation method, easy operation, low cost and high repeatability.
Description
Technical Field
The invention relates to the technical field of corrosion protection, in particular to Ni-WS2A preparation method of the plating layer.
Background
Nickel plating is one of the major alternatives to hard chrome plating and has been widely used today, for example: the nickel coating can be used as an anticorrosive material to improve the anticorrosive performance of metal, can also be used as a superhard wear-resistant material to improve the wear-resistant performance of a substrate, and can also be used for simply beautifying and decorating the substrate.
With the progress of science and technology, a single pure nickel coating cannot meet the development requirement. Although the surface performance of the substrate can be improved to a certain extent by the pure nickel coating, the dry friction coefficient of the pure nickel coating is high and is usually between 0.4 and 0.7, which is not beneficial to surface lubrication, and the hardness, wear resistance and corrosion resistance of the pure nickel coating cannot meet the use requirements of modern industry, which severely limits the application range of the nickel coating.
In the prior art, X100 pipeline steel in service for a long time is seriously corroded and needs surface anticorrosion treatment, but the prior corrosion protection technology of the X100 pipeline steel has the problems of poor corrosion resistance, high preparation cost and poor durability.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a Ni-WS2The preparation method of the coating can prepare a protective layer with excellent corrosion resistance on the surface of the X100 pipeline steel, not only greatly enhances the corrosion resistance and the durability of the X100 pipeline steel, but also has simple preparation method, easy operation, low cost and high repeatability.
The purpose of the invention is realized by the following technical scheme:
Ni-WS2The preparation method of the coating comprises the following steps:
step 2, mixing deionized water, nickel sulfate, nickel chloride and boric acid, adjusting the pH value of the mixed solution to 3.3-3.7, and adding cetyl trimethyl ammonium bromide, saccharin, tungsten disulfide nanoparticles, a brightener and a wetting agent to obtain an electroplating solution;
Preferably, the concentration of nickel sulfate in the electroplating solution is 250g/L, the concentration of nickel chloride is 45g/L, the concentration of boric acid is 40g/L, the concentration of cetyl trimethyl ammonium bromide is 0.1g/L, the concentration of saccharin is 1.5g/L, and the concentration of tungsten disulfide nanoparticles is 10 g/L.
Preferably, the grinding, polishing, cleaning and drying of the X100 pipeline steel comprises: grinding X100 pipeline steel on 800#, 1000#, 1200#, 1500# silicon carbide abrasive paper in sequence, then polishing by adopting polishing solution, then cleaning by adopting deionized water and acetone in sequence, removing surface grease mixture, then dropping anhydrous ethanol solution on the X100 pipeline steel, removing surface moisture, and then air-drying the X100 pipeline steel, thereby obtaining an X100 matrix.
According to the technical scheme provided by the invention, the nickel sulfate, the nickel chloride, the boric acid, the hexadecyl trimethyl ammonium bromide, the saccharin, the tungsten disulfide nano particles, the brightening agent and the wetting agent in a specific ratio are mixed to be used as the electroplating solution, and the electroplating solution is used for electroplating deposition, so that the Ni-WS with excellent corrosion resistance is prepared on the surface of the X100 pipeline steel2The coating not only greatly enhances the corrosion resistance and the durability of the X100 pipeline steel, but also has simple preparation method, easy operation, low cost and high repeatability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 shows X100 matrix and Ni-WS in example 1 of the present invention2And (4) a macro topography of the plating layer.
FIG. 2 shows Ni-WS in example 1 of the present invention2SEM topography and coating thickness of the coating.
FIG. 3 shows Ni-WS-containing belts in example 1 of the present invention2XRD pattern of X100 pipeline steel surface of the coating.
FIG. 4 shows a Ni-WS band in example 1 of the present invention2Open circuit test results for plated X100 pipeline steel versus uncoated X100 pipeline steel of the prior art.
FIG. 5 shows a Ni-WS band in example 1 of the present invention2And the electrochemical impedance spectrum test results of the X100 pipeline steel plated with the coating and the X100 pipeline steel which is not plated with the coating in the prior art are shown.
FIG. 6 shows a Ni-WS band in example 1 of the present invention2And the potentiodynamic polarization curve test result graphs of the X100 pipeline steel with the coating and the X100 pipeline steel without the coating in the prior art.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The following Ni-WS provided by the present invention2The method of preparing the plating layer is described in detail. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
Ni-WS2The preparation method of the coating comprises the following steps:
And 2, mixing deionized water, nickel sulfate, nickel chloride and boric acid, adjusting the pH value of the mixed solution to 3.3-3.7, and adding cetyl trimethyl ammonium bromide, saccharin, tungsten disulfide nanoparticles (the particle size of the tungsten disulfide nanoparticles is preferably 40nm), a brightener and a wetting agent to obtain the electroplating solution. The concentration of nickel sulfate in the electroplating solution is 250g/L, the concentration of nickel chloride is 45g/L, the concentration of boric acid is 40g/L, the concentration of cetyl trimethyl ammonium bromide is 0.1g/L, the concentration of saccharin is 1.5g/L, and the concentration of tungsten disulfide nano particles is 10 g/L.
In particular to Ni-WS provided by the invention2The preparation method of the coating has at least the following advantages:
(1) Ni-WS of the invention2Coating adopts WS2Nanoparticles, in comparison to other solid lubricant particles (e.g. MoS)2) Exhibits higher thermal stability and stronger oxidation resistance at medium and high temperatures; WS in comparison with other ceramic nanoparticles2When the nano particles and the metal salt are co-deposited, irregular protrusions are formed on the surface, so that the prepared plating layer shows a lotus leaf effect, and the plating layer has an anti-corrosion and anti-fouling function and a certain self-cleaning function; WS2The nanoparticles can improve the finish of the coating, reduce the friction resistance between the fluid and the wall surface of the coating, and integrally improve the corrosion resistance of the coating, wherein WS is used for improving the corrosion resistance of the coating2The surface of the formed composite coating layer is protruded with fullerene-likeThe corrosion resistance of the nickel-based alloy is higher than that of a pure nickel coating, and the nickel-based alloy is suitable for severe environments. Ni-WS prepared on X100 pipeline steel surface2The coating has hydrophobicity, namely the so-called lotus effect, and the multilayer surface appearance of the micron-nanometer structure enables the coating to have the characteristics of corrosion resistance, pollution prevention, ice prevention, self cleaning, oil-water separation and friction resistance reduction, and the coating is convenient to prepare, low in cost, low in energy consumption and has potential application prospects.
(2) The invention adopts the electroplating deposition technology to prepare Ni-WS on the surface of X100 pipeline steel2The coating can effectively solve the problems of high preparation cost and poor durability of an organic layer in the existing corrosion protection technology, and has the advantages of easy operation, low cost and high repeatability.
(3) Ni-WS in the present invention2The coating forms large area WS on the surface of the X100 pipeline steel2Nanoparticles, whereas WS2The nano particles have high thermal stability and good oxidation resistance, and are helpful for forming irregular bulges on the surface, so that the corrosion resistance of the X100 pipeline steel can be greatly enhanced.
(4) The requirement of super-hydrophobicity of the coating is to have a multi-layer surface topography, which is a micro-nano structure. The content of tungsten disulfide nanoparticles in the electroplating solution is a key factor for preparing the super-hydrophobic coating; the invention controls the content of the tungsten disulfide nano particles in the electroplating solution, thereby leading the Ni-WS prepared on the surface of the X100 pipeline steel2The coating becomes a super-hydrophobic coating and has the effects of corrosion resistance, pollution resistance and self-cleaning.
(5) The electroplating deposition process is completed in electroplating solution containing 10g/L tungsten disulfide nano particles, and the preparation method has the advantages of one-step preparation, time saving and no need of low-surface-energy organic matter modification.
(6) The electroplating solution of the present invention has brightener and wetting agent added to raise Ni-WS content2The brightness of the plating layer.
In conclusion, the protective layer with excellent corrosion resistance can be prepared on the surface of the X100 pipeline steel, so that the corrosion resistance and the durability of the X100 pipeline steel are greatly enhanced, and the preparation method is simple, easy to operate, low in cost and high in repeatability.
In order to more clearly show the technical solutions and the technical effects provided by the present invention, the following embodiments are provided to illustrate the Ni-WS provided by the embodiments of the present invention2The method of preparing the plating layer is described in detail.
Example 1
Ni-WS2The preparation method of the coating comprises the following steps:
preparation of (I) X100 substrates
Grinding 15X 15mm X100 pipeline steel on 800#, 1000#, 1200# and 1500# silicon carbide abrasive paper in sequence, polishing after the grinding effect reaches no large-area scratches, dropping polishing liquid for polishing during polishing, then cleaning by deionized water and acetone in sequence, removing surface grease mixture, dropping anhydrous ethanol solution on the X100 pipeline steel, removing surface moisture, then drying the X100 pipeline steel by electric heating, sealing by a sealing bag, preventing surface oxidation, and thus obtaining the X100 matrix.
(II) preparing electroplating solution and adjusting the pH value of the electroplating solution
The preparation method of the electroplating solution comprises the following steps: adding 50g of nickel sulfate, 9g of nickel chloride and 8g of boric acid into deionized water, mixing and stirring uniformly, adjusting the pH value of the mixed solution to 3.3-3.7 by using dilute hydrochloric acid or sodium hydroxide, then adding 0.02g of hexadecyl trimethyl ammonium bromide, 2g of saccharin and 0.3g of tungsten disulfide nanoparticles, and then injecting 0.05mL of brightener and 0.24mL of wetting agent into the mixed solution by using a needle syringe so as to obtain 200mL of electroplating solution.
The plating solution needs to be replaced every time of plating, and the plating solution can not be used continuously overnight.
(III) preparation of Ni-WS2Coating layer
Adopting a direct current stabilized voltage supply to supply power, taking a pure nickel sheet as an anode and the X100 substrate as a cathode, wherein the area of the pure nickel sheet is slightly larger than that of the X100 substrate, placing the anode and the cathode in the electroplating solution to carry out electroplating deposition, and the current density is 4A/dm2At a current of 009A, electroplating deposition time is 35 minutes, thereby obtaining Ni-WS on the surface of X100 pipeline steel2And (7) plating.
Will carry Ni-WS2Cleaning the surface of the plated X100 pipeline steel with deionized water to remove the electroplating solution on the surface of the X100 pipeline steel, and then performing electric heating air drying to obtain a clean Ni-WS-bearing steel2Coated X100 pipeline steel.
Morphology observation and performance detection
For the X100 matrix and Ni-WS in the example 1 of the present invention2The following appearance observation and performance detection are carried out on the plating layer:
(1) scanning electron microscope was used to align X100 substrate and Ni-WS in inventive example 12Carrying out appearance observation and thickness characterization on the coating to obtain an X100 matrix and Ni-WS shown in figure 12Macroscopic topography of the coating and Ni-WS as shown in FIG. 22SEM topography map and cladding thickness map of the cladding; wherein, FIG. 1(a) is the macro topography of X100 matrix in the example 1 of the present invention, and FIG. 1(b) is the Ni-WS in the example 1 of the present invention2FIG. 2(a) is a macro-topographic map of the plated layer, which is Ni-WS in example 1 of the present invention2SEM topography of the plating layer, FIG. 2(b) is the Ni-WS2Coating thickness of the coating. As can be seen from fig. 1 and 2: the spherical substances in the figure 2(a) are different in size and are mutually aggregated to form an agglomeration phenomenon, the appearance is similar to that observed macroscopically in the figure 1(b), and it is inferred that the electroplating process can cause the agglomeration phenomenon of the coating metal, so that the surface of the X100 pipeline steel has obvious rough feeling. As can be seen from fig. 2 (a): during the regeneration process of the coating metal on the surface of the X100 pipeline steel, two or more crystal grains are gathered together, and as the electroplating time is increased, the crystal grains are rapidly increased and are continuously combined with other crystal grains or crystal grain groups to form larger crystal grain groups. As can be seen from fig. 2 (b): Ni-WS of X100 pipeline steel surface2Relatively flat and uniform coating, Ni-WS2The thickness of the coating is approximately 34 μm in the Ni-WS range2A gap of 7-8 μm is formed between the plating layer and the X100 substrate.
(2) X-ray diffractometer for Ni-WS in inventive example 12Coating for object image compositionAnd analyzed to obtain an X-ray diffraction pattern (XRD pattern) as shown in FIG. 3. As can be seen from fig. 3: the main phases being Fe, Ni and WS2. Fe from X100 pipeline steel substrate, Ni and WS2The appearance of diffraction peaks indicates Ni2+Fully participate in the electrochemical reaction, WS2The nano particles are uniformly dispersed in the coating and combined with the replaced Ni simple substance.
(3) For the Ni-WS-bearing band in the embodiment 1 of the invention2The coated X100 pipeline steel and the X100 pipeline steel which is not coated in the prior art are respectively subjected to an open circuit test, so as to obtain an open circuit test result chart shown in fig. 4; wherein FIG. 4(a) shows a Ni-WS band in example 1 of the present invention2FIG. 4(b) is a graph showing the results of open circuit test after soaking the X100 pipe steel coated with the coating layer and the X100 pipe steel uncoated with the prior art for 0.5h, in example 1 of the present invention2And (3) a graph of open circuit test results after soaking the X100 pipeline steel plated with the coating and the X100 pipeline steel uncoated with the coating for 24 hours in the prior art. As can be seen from fig. 4: soaking for 0.5h, and then carrying Ni-WS2The open circuit potential of the X100 pipeline steel with the coating is-0.438V, and the open circuit potential of the X100 pipeline steel without the coating is-0.75V; soaking for 24h, and then carrying Ni-WS2The open circuit potential of the X100 pipeline steel of the coating is-0.693V, and the open circuit potential of the X100 pipeline steel without the coating is-0.721V; with Ni-WS2The open circuit potential value of the X100 pipeline steel coated is obviously higher than that of the X100 pipeline steel not coated, which shows that the Ni-WS of the invention2The plating layer tends to have good corrosion resistance.
(4) For the Ni-WS-bearing band in the embodiment 1 of the invention2Respectively carrying out electrochemical impedance spectroscopy test on the X100 pipeline steel with the coating and the X100 pipeline steel without the coating in the prior art, thereby obtaining a test result chart of the electrochemical impedance spectroscopy shown in FIG. 5; wherein FIG. 5(a) shows a Ni-WS band in example 1 of the present invention2Bode diagram of the X100 pipeline steel coated with Ni-WS and the X100 pipeline steel uncoated with the prior art, FIG. 5(b) is the Bode diagram of the pipeline steel with Ni-WS in example 1 of the present invention2Nyquist plots for the coated X100 line steel versus the uncoated X100 line steel of the prior art. As can be seen from fig. 5: bode with Ni-WS in the diagram2Of coated X100 pipeline steelThe resistance value is higher than that of X100 pipeline steel without coating, and Ni-WS is carried in a Nyquist diagram2The coated X100 pipeline steel has a larger capacitive arc radius than the uncoated X100 pipeline steel, and the larger the capacitive arc radius, the larger the resistance and the more corrosion resistant, which indicates that the steel is coated with Ni-WS2The coated X100 pipeline steel is more corrosion resistant than the uncoated X100 pipeline steel.
(5) For the Ni-WS-bearing band in the embodiment 1 of the invention2Performing potentiodynamic polarization curve test on the X100 pipeline steel with the coating and X100 pipeline steel without the coating in the prior art respectively to obtain a potentiodynamic polarization curve test result chart shown in FIG. 6; wherein, FIG. 6(a) shows a Ni-WS band in example 1 of the present invention2FIG. 6(b) is a graph showing the results of potentiodynamic polarization curve tests of the X100 pipe steel coated with the coating and the X100 pipe steel uncoated with the prior art after soaking for 0.5h, in example 1 of the present invention2And the potentiodynamic polarization curve test result chart of the X100 pipeline steel of the coating and the X100 pipeline steel without the coating in the prior art after being soaked for 24 hours. As can be seen from fig. 5: with Ni-WS in example 1 of the present invention2The X100 pipeline steel with the coating and the X100 pipeline steel without the coating in the prior art are respectively soaked in the corrosive liquid of the produced water of the oil field for 0.5h and 24h, and the result shows that the steel has Ni-WS2The corrosion current density of the coated X100 pipeline steel is from 2.64 mu A/cm2Change to 12.6. mu.A/cm2The corrosion current density of the X100 pipeline steel without coating is from 211 mu A/cm2Change to 196. mu.A/cm2This indicates that as the corrosion time progresses, corrosion products begin to appear and the corrosion resistance is reduced, but with Ni-WS2The corrosion current density of the X100 pipeline steel with the coating is much smaller than that of the X100 pipeline steel without the coating, the phase difference is two orders of magnitude after soaking for 0.5h, and the phase difference is one order of magnitude after soaking for 24h, which reflects that the steel with the Ni-WS2The X100 pipeline steel of the coating is more corrosion-resistant, and the corrosion influence is effectively reduced.
With Ni-WS in example 1 of the present invention2The EIS fitting results of the coated X100 pipeline steel and the uncoated X100 pipeline steel of the prior art after 0.5h immersion and 24h immersion, respectively, are shown in table 1 below:
TABLE 1
With Ni-WS in example 1 of the present invention2The results of the polarization curve fitting of the coated X100 pipeline steel and the uncoated X100 pipeline steel of the prior art after soaking for 0.5h and soaking for 24h are shown in table 2 below:
TABLE 2
In conclusion, the protective layer with excellent corrosion resistance can be prepared on the surface of the X100 pipeline steel, so that the corrosion resistance and the durability of the X100 pipeline steel are greatly enhanced, and the preparation method is simple, easy to operate, low in cost and high in repeatability.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. Ni-WS2The preparation method of the coating is characterized by comprising the following steps:
step 1, grinding, polishing, cleaning and drying X100 pipeline steel to obtain an X100 matrix;
step 2, mixing deionized water, nickel sulfate, nickel chloride and boric acid, adjusting the pH value of the mixed solution to 3.3-3.7, and adding cetyl trimethyl ammonium bromide, saccharin, tungsten disulfide nanoparticles, a brightener and a wetting agent to obtain an electroplating solution;
step 3, adopting a direct current stabilized power supply to supply power, taking a pure nickel sheet as an anode and the X100 substrate as a cathode, and carrying out electroplating deposition in the electroplating solution, wherein the current density is 4A/dm2The current is 0.09A, and the electroplating deposition time is 30-40 minutes, so that Ni-WS is prepared on the surface of the X100 pipeline steel2And (7) plating.
2. Ni-WS according to claim 12The preparation method of the plating layer is characterized in that the concentration of nickel sulfate in the electroplating solution is 250g/L, the concentration of nickel chloride is 45g/L, the concentration of boric acid is 40g/L, the concentration of cetyl trimethyl ammonium bromide is 0.1g/L, the concentration of saccharin is 1.5g/L, and the concentration of tungsten disulfide nanoparticles is 10 g/L.
3. Ni-WS according to claim 1 or 22The preparation method of the coating is characterized in that the steps of grinding, polishing, cleaning and drying the X100 pipeline steel comprise:
grinding X100 pipeline steel on 800#, 1000#, 1200#, 1500# silicon carbide abrasive paper in sequence, then polishing by adopting polishing solution, then cleaning by adopting deionized water and acetone in sequence, removing surface grease mixture, then dropping anhydrous ethanol solution on the X100 pipeline steel, removing surface moisture, and then air-drying the X100 pipeline steel, thereby obtaining an X100 matrix.
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