CN105568243A - Preparing method of graphene anticorrosive coating for stainless steel surface - Google Patents
Preparing method of graphene anticorrosive coating for stainless steel surface Download PDFInfo
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- CN105568243A CN105568243A CN201610148083.8A CN201610148083A CN105568243A CN 105568243 A CN105568243 A CN 105568243A CN 201610148083 A CN201610148083 A CN 201610148083A CN 105568243 A CN105568243 A CN 105568243A
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- graphene
- stainless steel
- ion sputtering
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- corrosion protection
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/46—Sputtering by ion beam produced by an external ion source
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
Abstract
The invention belongs to the technical field of carbon nano materials, and relates to a preparing method of a graphene anticorrosive coating for a stainless steel surface. Natural graphite serves as a raw material, graphene powder is prepared through an oxidation-reduction method, and then is subject to freeze drying for standby application, the graphene powder is put in a piece pressing machine to be pressed into a graphene thin film, then the graphene thin film is placed above a stainless steel substrate, and serves as an ion sputtering target material, a high-energy ion gun is adopted to perform ion sputtering on the graphene thin film, and through ion sputtering, the graphene thin film is broken and therefore is evenly deposited on the surface of a stainless steel sample in a covering manner, and the graphene anticorrosive coating is prepared on the surface of the stainless steel sample; and the prepared graphene anticorrosive coating is uniform, the thickness of the coating is easily controlled, a used device is simple, the preparing efficiency is high, energy consumption is low, and the anticorrosive performance is excellent.
Description
Technical field:
The invention belongs to carbon nanomaterial preparation technology field, relate to the technique that a kind of ion sputtering process prepares Graphene corrosion protection coating, particularly a kind of Graphene corrosion protection coating preparation method for stainless steel surface, the Graphene coating antiseptic excellent performance of preparation.
Background technology:
Graphene is a kind of new carbon, there is excellent heat conduction and electroconductibility, high transmission rate, high strength, also there is the many advantages such as abundant raw material, toxicity are little, biocompatibility, in fields such as pharmaceutical carrier, energy storage, sensor preparation, optics, catalysis, there is great using value.Stainless steel has the excellent characteristic such as good intensity, higher wear resistance, is therefore widely used in pipeline, public utility, all respects of the life such as motorway.Annual China is because of Corrosion of Stainless Steel, and the financial loss suffered is up to exceeding 100 billion, and the antiseptic property therefore carrying out hardened stainless steel by coating reduces financial loss becomes a kind of requisite measure.A lot of about the report of hardened stainless steel antiseptic property method at present, mainly comprise zinc, chromium, clay-like material coated etc., these materials be employed often have certain injury to environment and human body or have water-absorbent, are generally difficult to realize application on a large scale with anticorrosion efficiently.Therefore, the high efficiency coating preparation exploring a kind of quick, simple, cheap, nontoxic, isolated water and air is necessary very much, ion sputtering process has device relative to other methods such as electrochemical processes and the advantage such as making processes is simple, it is the very important method of the one preparing high-quality thin film grown up in recent years, it has the incomparable advantage of other technology, in film-forming process, sedimentation velocity is slow, the thickness of film and quality easily control.Therefore, the preparation of the antiseptic property that comprehensive grapheme material itself is excellent and ion sputtering process high-quality thin film, seek a kind of Graphene corrosion protection coating preparation method for stainless steel surface, in the preparation process of coating, graphene sheet layer is broken and diminishes, the dense packing of higher degree can be realized, make stainless steel reach efficient water proof and exhausted gas.
Summary of the invention:
The object of the invention is to the shortcoming overcoming prior art and starting material existence, seeking to design provides a kind of Graphene corrosion protection coating preparation method for stainless steel surface, Graphene corrosion protection coating is prepared based on ion sputtering process, the Graphene corrosion protection coating prepared has the advantages such as stable, efficient, toxicity is little, isolated water and air, can the antiseptic property of hardened stainless steel.
To achieve these goals, the technique that the present invention prepares Graphene corrosion protection coating specifically comprises the following steps:
(1), take natural graphite as raw material, graphene powder is prepared by oxidation reduction process, then lyophilize is carried out to graphene powder, first by 0.1g graphite, 0.3g potassium permanganate, within 12 hours, graphite oxide is obtained 30 degrees Celsius of reactions with after the mixing of the 90ml vitriol oil, be dissolved in 200ml distilled water by after the graphite oxide centrifuge washing obtained, then 100 microlitre hydrazine hydrates are added, after 95 degrees Celsius of lower reductase 12s hour, centrifugal, lyophilize is carried out to the sample obtained, obtain graphene powder;
(2), by graphene powder be placed in tabletting machine, with the pressure of 30Mpa, graphene powder be pressed into graphene film;
(3), graphene film prepared by step (2) is placed on the top at the stainless steel-based end, graphene film is as the target of ion sputtering, energetic ion rifle is adopted to carry out ion sputtering to graphene film, after ion sputtering, the broken thus uniform deposition of graphene film covers the surface of stainless steel sample, Graphene corrosion protection coating is obtained at stainless steel sample surfaces, wherein the acceleration voltage of ion sputtering is set to 300V, and in deposition process, the air pressure of argon gas and flow velocity are respectively 0.04Pa and 4cm
3/ min, sputtering time is set to 1h, 2h, 3h or 5h.
Oxidation style of the present invention is the HUMMERS method improved, and reduction method is thoroughly reduced by hydrazine hydrate reduction agent.
The present invention is by adopting means of different to characterize to the Graphene corrosion protection coating of gained, and the means adopted comprise scanning electronic microscope (SEM), x-ray photoelectron spectroscopy (XPS).
The present invention passes through electrochemical workstation, with the electrochemical method such as polarization curve and electrochemical impedance, the antiseptic property of material is detected, there is the polarization curve forward migration of the sample of Graphene corrosion protection coating, corrosion current reduces, and simultaneous electrochemical impedance becomes large, and this shows the raising of antiseptic property, stainless erosion rate is reduced to 0.00138mm/year by 0.019mm/year, reduces 12.76 times.
The present invention compared with prior art, has the following advantages: one is that the Graphene corrosion protection coating of preparation is even, and thickness is easy to control, and the device of use is simple; Two is that preparation efficiency is high, and the time completing primary first-order equation is shorter, only needs 30-60min; Three is that energy consumption is low, and Graphene makes low in raw material price, and ion sputtering energy consumption is low; Four is that Graphene corrosion protection coating is piled up closely at stainless steel surface, and antiseptic property is superior, and erosion rate is reduced to 0.00138mm/year by 0.019mm/year, reduces 12.76 times, and stainless steel preservative efficiency can keep more than 90%; Five is strengthenings Graphene corrosion protection coating being applied to stainless steel antiseptic property, and preparation is stable, and can reappear, efficiency is high, and the carbon quantum dot quality of preparation is good, stable performance.
Accompanying drawing illustrates:
Fig. 1 is the apparatus structure principle schematic that the present invention prepares Graphene corrosion protection coating, comprising energetic ion rifle, graphene film, the stainless steel-based end.
Fig. 2 is that SEM figure (D) of Graphene corrosion protection coating prepared by the present invention, pure stainless SEM figure (A and B) and stainless steel surface have corrosion protection coating and do not have the comparison diagram (C) of corrosion protection coating.
Fig. 3 is the XPS figure of the stainless steel sample with Graphene corrosion protection coating prepared of the present invention and pure stainless steel sample.
Fig. 4 is stainless steel sample and pure stainless steel sample TAFEL graphic representation (A), erosion rate figure (B), open circuit voltage figure (C) and the preservative efficiency figure (D) that the embodiment of the present invention has corrosion protection coating.
Embodiment:
Below by embodiment, also the invention will be further described by reference to the accompanying drawings.
Embodiment 1:
The technique that the present embodiment prepares Graphene corrosion protection coating specifically comprises the following steps:
(1), take natural graphite as raw material, graphene powder is prepared by oxidation reduction process, then lyophilize is carried out to graphene powder, first by 0.1g graphite, 0.3g potassium permanganate, within 12 hours, graphite oxide is obtained 30 degrees Celsius of reactions with after the mixing of the 90ml vitriol oil, be dissolved in 200ml distilled water by after the graphite oxide centrifuge washing obtained, then 100 microlitre hydrazine hydrates are added, after 95 degrees Celsius of lower reductase 12s hour, centrifugal, lyophilize is carried out to the sample obtained, obtain graphene powder;
(2), by graphene powder be placed in tabletting machine, with the pressure of 30Mpa, graphene powder be pressed into graphene film;
(3), graphene film prepared by step (2) is placed on the top at the stainless steel-based end, graphene film is as the target of ion sputtering, energetic ion rifle is adopted to carry out ion sputtering to graphene film, after ion sputtering, the broken thus uniform deposition of graphene film covers the surface of stainless steel sample, Graphene corrosion protection coating is obtained at stainless steel sample surfaces, wherein the acceleration voltage of ion sputtering is set to 300V, and in deposition process, the air pressure of argon gas and flow velocity are respectively 0.04Pa and 4cm
3/ min.
The time that the present embodiment controls ion sputtering is respectively 2h, 3h and 5h, thus realizes the control of corrosion protection coating thickness, and experimental result shows, and during 3h, corrosion protection coating appropriate thickness, preservative effect reaches best effect.
Claims (1)
1., for a Graphene corrosion protection coating preparation method for stainless steel surface, it is characterized in that specifically comprising the following steps:
(1), take natural graphite as raw material, graphene powder is prepared by oxidation reduction process, then lyophilize is carried out to graphene powder, first by 0.1g graphite, 0.3g potassium permanganate, within 12 hours, graphite oxide is obtained 30 degrees Celsius of reactions with after the mixing of the 90ml vitriol oil, be dissolved in 200ml distilled water by after the graphite oxide centrifuge washing obtained, then 100 microlitre hydrazine hydrates are added, after 95 degrees Celsius of lower reductase 12s hour, centrifugal, lyophilize is carried out to the sample obtained, obtain graphene powder;
(2), by graphene powder be placed in tabletting machine, with the pressure of 30Mpa, graphene powder be pressed into graphene film;
(3), graphene film prepared by step (2) is placed on the top at the stainless steel-based end, graphene film is as the target of ion sputtering, energetic ion rifle is adopted to carry out ion sputtering to graphene film, after ion sputtering, the broken thus uniform deposition of graphene film covers the surface of stainless steel sample, Graphene corrosion protection coating is obtained at stainless steel sample surfaces, wherein the acceleration voltage of ion sputtering is set to 300V, and in deposition process, the air pressure of argon gas and flow velocity are respectively 0.04Pa and 4cm
3/ min, sputtering time is set to 1h, 2h, 3h or 5h.
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| CN105568243B CN105568243B (en) | 2018-04-20 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105908053A (en) * | 2016-05-27 | 2016-08-31 | 天津平高智能电气有限公司 | Graphene-stainless steel composite material and preparation method and application thereof |
| CN106784915A (en) * | 2016-11-30 | 2017-05-31 | 哈尔滨工业大学 | A kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating |
| CN109208044A (en) * | 2018-11-05 | 2019-01-15 | 山东科技大学 | A kind of layered bionic wear-and corrosion-resistant anti-friction coating and preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105908053A (en) * | 2016-05-27 | 2016-08-31 | 天津平高智能电气有限公司 | Graphene-stainless steel composite material and preparation method and application thereof |
| CN106784915A (en) * | 2016-11-30 | 2017-05-31 | 哈尔滨工业大学 | A kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating |
| CN109208044A (en) * | 2018-11-05 | 2019-01-15 | 山东科技大学 | A kind of layered bionic wear-and corrosion-resistant anti-friction coating and preparation method and application |
| CN109208044B (en) * | 2018-11-05 | 2020-06-09 | 山东科技大学 | Layered bionic wear-resistant corrosion-resistant antifriction coating and preparation method and application thereof |
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| CN105568243B (en) | 2018-04-20 |
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Effective date of registration: 20210106 Address after: 221000 Shimao Square Inner Commercial Street 2, Office 1, Office 2, Building 1-910, Yunlong District, Xuzhou City, Jiangsu Province Patentee after: Jiangsu Shifeng Enterprise Management Consulting Co.,Ltd. Address before: Room 104, experimental area 1, Linyi University, middle section of Shuangling Road, Lanshan District, Linyi City, Shandong Province 276005 Patentee before: LINYI University |
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