CN111763974A - Preparation method of graphene-based super-hydrophobic stainless steel - Google Patents
Preparation method of graphene-based super-hydrophobic stainless steel Download PDFInfo
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- CN111763974A CN111763974A CN201910257328.4A CN201910257328A CN111763974A CN 111763974 A CN111763974 A CN 111763974A CN 201910257328 A CN201910257328 A CN 201910257328A CN 111763974 A CN111763974 A CN 111763974A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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Abstract
The invention belongs to the technical field of functional materials, and relates to a preparation method of graphene-based super-hydrophobic stainless steel. The invention provides a preparation method of graphene-based super-hydrophobic stainless steel, and particularly relates to a preparation method of a super-hydrophobic structure by adopting an electrodeposition method. Has the following advantages: on one hand, the stainless steel is etched in a linolenic acid medium to construct a rough structure on the surface of the stainless steel, on the other hand, the lamellar blocking function of the graphene is fully exerted, the corrosion inhibition efficiency reaches more than 97 percent, and the corrosion inhibition method has wide industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a preparation method of graphene-based super-hydrophobic stainless steel.
Background
Stainless steel is a general metal material, and has good corrosion resistance, heat resistance, low-temperature strength and mechanical properties, good hot workability such as stamping and bending, and no hot treatment hardening phenomenon, so that the stainless steel is widely applied to the fields of chemical industry, electric power, navigation, weaponry and the like to manufacture machines and parts such as heat exchange equipment, containers, valves, pumps, turbines, shafts and the like. However, when exposed to corrosive media, particularly chloride ion-containing environments, severe corrosion can occur.
In recent years, inspired by the lotus effect, the super-hydrophobic surface with a contact angle of more than 150 degrees with a water drop has the strong hydrophobic characteristic that water molecules and corrosive ions are difficult to permeate into the super-hydrophobic surface, so that the corrosion resistance of the metal material is obviously improved.
At present, a super-hydrophobic structure is constructed on the surface of a metal material by the etching action of stearic acid on the metal material, but the super-hydrophobic structure has short service life and is easy to damage after being soaked in a corrosive medium for a long time. The preparation method of the super-hydrophobic surface reported at present either needs harsh equipment or has too long preparation time. Therefore, the preparation method of the simple, high-efficiency and long-life super-hydrophobic stainless steel has important economic significance and social significance.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for preparing a quick and long-life super-hydrophobic stainless steel, and the super-hydrophobic structure constructed by the method is stable and is particularly suitable for protecting 304 stainless steel in a 3.5% NaCl solution corrosion medium.
The invention provides a preparation method of graphene-based super-hydrophobic stainless steel, which comprises the following steps:
(1) pretreatment of stainless steel:
the stainless steel is firstly polished by 60-mesh, 120-mesh, 320-mesh, 600-mesh and 1200-mesh sandpaper respectively to remove impurities and oxides on the surface, then ultrasonically cleaned by absolute ethyl alcohol and acetone for 10 minutes to remove organic matters, and finally subjected to N treatment2Drying for later use;
(2) preparing a super-hydrophobic structure by electrodeposition:
the electrolyte formula consists of graphene oxide, linolenic acid and absolute ethyl alcohol, and the mass fractions of the graphene oxide, the linolenic acid and the absolute ethyl alcohol are respectively as follows: 15-30% of graphene oxide, 25-40% of linolenic acid and 40-70% of absolute ethyl alcohol, wherein the sum of the percentage contents of all the components is 100%. The preparation method of the super-hydrophobic stainless steel provided by the invention has the advantages that the constant potential is 5-20V, the electrodeposition time is 4-12 h, and the temperature is 30-50 ℃. On one hand, the invention utilizes linolenic acid to etch the stainless steel; on the other hand, a film layer with high blocking performance is formed by utilizing the strong adsorption force of the graphene oxide on the surface of the stainless steel, so that a super-hydrophobic surface is constructed, and the super-hydrophobic stainless steel has excellent corrosion resistance. The preparation process is simple, the reproducibility is good, expensive equipment is not needed, and the method has wide industrial application prospect.
The invention has the beneficial effects that:
1. the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, which can obviously improve the corrosion resistance of 304 stainless steel in a 3.5% NaCl solution corrosion medium;
2. the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, wherein linolenic acid and graphene oxide are adopted as electrolyte, and the obtained film layer has better super-hydrophobic performance;
3. the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, which has lower applied voltage and can effectively reduce energy consumption;
4. the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, which has short electrodeposition time, and can construct a super-hydrophobic surface in only 6 hours under the voltage of 10V;
5. the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, and the super-hydrophobic membrane has longer service life;
6. the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, which not only has a super-hydrophobic structure, but also has excellent corrosion resistance, and has excellent protection effect on 304 stainless steel in a 3.5% NaCl solution corrosion medium;
7. the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, wherein the preparation method is simple, the energy consumption is low, and the electrolyte formula is non-toxic and pollution-free and can be applied to large-scale industrial application.
Drawings
FIG. 1: contact angle of untreated 304 stainless steel;
FIG. 2: contact angle of graphene-based superhydrophobic 304 stainless steel;
FIG. 3: the polarization curve test result of untreated 304 stainless steel in 3.5% NaCl solution corrosion medium;
FIG. 4: and (3) curve test results of the graphene-based super-hydrophobic 304 stainless steel in a 3.5% NaCl solution corrosion medium.
Detailed Description
The invention is further described below with reference to the figures and examples. While the invention will be described in conjunction with the preferred embodiments, it will be understood that they are not intended to limit the invention to the embodiments. On the contrary, the invention is intended to cover alternatives, modifications and equivalents, which may be included within the scope of the invention as defined by the appended claims.
Example 1:
the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, which comprises the following steps:
(1) pretreatment of stainless steel:
the stainless steel is firstly respectively passed through 60 meshesSanding 120-mesh, 320-mesh, 600-mesh and 1200-mesh sandpaper to remove impurities and oxides on the surface, ultrasonically cleaning with absolute ethyl alcohol and acetone for 10 minutes to remove organic matters, and then performing N-ultrasonic cleaning2Drying for later use;
(2) preparing a super-hydrophobic structure by electrodeposition:
the electrolyte formula consists of graphene oxide, linolenic acid and absolute ethyl alcohol, and the mass fractions of the graphene oxide, the linolenic acid and the absolute ethyl alcohol are respectively as follows: 15% of graphene oxide, 25% of linolenic acid and 60% of absolute ethyl alcohol. The preparation method of the super-hydrophobic stainless steel provided by the invention has the advantages that the constant potential is 5V, the electrodeposition time is 10 h, and the temperature is 50 ℃.
The contact angle of the prepared graphene-based super-hydrophobic stainless steel is measured by a contact angle tester, and compared with the contact angle of the graphene-based super-hydrophobic stainless steel which is not subjected to super-hydrophobic treatment, the contact angle of the graphene-based super-hydrophobic stainless steel is higher than 150 degrees after the graphene-based super-hydrophobic stainless steel is treated by the method, and the result is shown in figures 1 and 2.
Example 2:
the invention provides a preparation method of graphene-based super-hydrophobic stainless steel, which comprises the following steps:
(1) pretreatment of stainless steel:
the stainless steel is firstly polished by 60-mesh, 120-mesh, 320-mesh, 600-mesh and 1200-mesh sandpaper respectively to remove impurities and oxides on the surface, then ultrasonically cleaned by absolute ethyl alcohol and acetone for 10 minutes to remove organic matters, and finally subjected to N treatment2Drying for later use;
(2) preparing a super-hydrophobic structure by electrodeposition:
the electrolyte formula consists of graphene oxide, linolenic acid and absolute ethyl alcohol, and the mass fractions of the graphene oxide, the linolenic acid and the absolute ethyl alcohol are respectively as follows: 30% of graphene oxide, 40% of linolenic acid and 30% of absolute ethyl alcohol. The preparation method of the super-hydrophobic stainless steel provided by the invention has the advantages that the constant potential is 20V, the electrodeposition time is 6 h, and the temperature is 30 ℃.
Electrochemical impedance test is carried out on the graphene-based super-hydrophobic stainless steel in a 3.5% NaCl solution corrosion medium, and compared with 304 stainless steel which is not subjected to super-hydrophobic treatment, the result is shown in fig. 3, fig. 4 and table 2, after the graphene-based super-hydrophobic stainless steel is treated by the method, the charge transfer resistance is obviously increased, and the prepared graphene-based super-hydrophobic stainless steel has better corrosion resistance.
TABLE 2
| Condition | Rct, Ω.cm2 | Corrosion inhibition efficiency% |
| Without super-hydrophobic treatment | 1642 | |
| Super-hydrophobic | 56467 | 97.1% |
Claims (8)
1. A preparation method of graphene-based super-hydrophobic stainless steel is characterized by comprising the following two steps:
(1) pretreatment of stainless steel:
the stainless steel is firstly polished by 60-mesh, 120-mesh, 320-mesh, 600-mesh and 1200-mesh sandpaper respectively to remove impurities and oxides on the surface, then ultrasonically cleaned by absolute ethyl alcohol and acetone for 10 minutes to remove organic matters, and finally subjected to N treatment2Drying for later use;
(2) preparing a super-hydrophobic structure by electrodeposition:
the electrolyte formula consists of graphene oxide, linolenic acid and absolute ethyl alcohol, and the mass fractions of the graphene oxide, the linolenic acid and the absolute ethyl alcohol are respectively as follows: 15-30% of graphene oxide, 25-40% of linolenic acid and 40-70% of absolute ethyl alcohol, wherein the sum of the percentage contents of all the components is 100%.
2. The preparation method of the graphene-based super-hydrophobic stainless steel provided by the invention comprises the steps of keeping the constant potential at 5-20V, carrying out electrodeposition for 4-12 h at 30-50 ℃, and obtaining the graphene super-hydrophobic stainless steel, wherein the super-hydrophobic stainless steel has excellent corrosion resistance in a 3.5% NaCl solution corrosion medium.
3. The method for preparing the graphene-based super-hydrophobic stainless steel according to claim 1, wherein the electrolyte formula consists of graphene oxide, linolenic acid and absolute ethyl alcohol.
4. The method for preparing the graphene-based super-hydrophobic stainless steel according to claim 1, wherein the stainless steel is firstly sanded by 60-mesh, 120-mesh, 320-mesh, 600-mesh and 1200-mesh sandpaper to remove impurities and oxides on the surface.
5. The method for preparing the graphene-based super-hydrophobic stainless steel according to claim 1, wherein the stainless steel after oil removal is subjected to N treatment2And drying for later use.
6. The method for preparing the graphene-based super-hydrophobic stainless steel according to claim 1, wherein the constant potential is 5-20V.
7. The method for preparing the graphene-based super-hydrophobic stainless steel according to claim 1, wherein the electrodeposition time is 4-12 h.
8. The method for preparing the graphene-based super-hydrophobic stainless steel according to claim 1, wherein the electrodeposition temperature is 30-50 ℃.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104005026A (en) * | 2014-05-20 | 2014-08-27 | 华南理工大学 | Method for preparing corrosion-resistant super-hydrophobic membrane layer on surface of magnesium alloy |
| CN104264196A (en) * | 2014-09-30 | 2015-01-07 | 华南理工大学 | Method for preparing super-hydrophobic membrane layer on surface of magnesium alloy through one-step method as well as alloy and application of uper-hydrophobic membrane layer |
| CN106148900A (en) * | 2016-08-03 | 2016-11-23 | 上海晶顿科技有限公司 | A kind of graphene oxide super-hydrophobic coat and evaporated device thereof |
| CN106693727A (en) * | 2017-01-09 | 2017-05-24 | 河北工业大学 | Preparation method of super-hydrophobic polyvinylidene fluoride microporous membrane |
| CN108641421A (en) * | 2018-05-22 | 2018-10-12 | 陕西科技大学 | A kind of preparation method of graphene-based self-repairing super hydrophobic coating |
| CN109355689A (en) * | 2018-12-11 | 2019-02-19 | 山东工商学院 | The method and its application of super-hydrophobic coat are prepared based on electrodeposition process |
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- 2019-04-01 CN CN201910257328.4A patent/CN111763974A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104005026A (en) * | 2014-05-20 | 2014-08-27 | 华南理工大学 | Method for preparing corrosion-resistant super-hydrophobic membrane layer on surface of magnesium alloy |
| CN104264196A (en) * | 2014-09-30 | 2015-01-07 | 华南理工大学 | Method for preparing super-hydrophobic membrane layer on surface of magnesium alloy through one-step method as well as alloy and application of uper-hydrophobic membrane layer |
| CN106148900A (en) * | 2016-08-03 | 2016-11-23 | 上海晶顿科技有限公司 | A kind of graphene oxide super-hydrophobic coat and evaporated device thereof |
| CN106693727A (en) * | 2017-01-09 | 2017-05-24 | 河北工业大学 | Preparation method of super-hydrophobic polyvinylidene fluoride microporous membrane |
| CN108641421A (en) * | 2018-05-22 | 2018-10-12 | 陕西科技大学 | A kind of preparation method of graphene-based self-repairing super hydrophobic coating |
| CN109355689A (en) * | 2018-12-11 | 2019-02-19 | 山东工商学院 | The method and its application of super-hydrophobic coat are prepared based on electrodeposition process |
Non-Patent Citations (1)
| Title |
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| 丁芳林: "《食品化学》", 31 January 2017, 华中科技大学电子音像出版社 * |
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