CN105568243B - A kind of graphene corrosion-inhibiting coating preparation method for stainless steel surface - Google Patents
A kind of graphene corrosion-inhibiting coating preparation method for stainless steel surface Download PDFInfo
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- CN105568243B CN105568243B CN201610148083.8A CN201610148083A CN105568243B CN 105568243 B CN105568243 B CN 105568243B CN 201610148083 A CN201610148083 A CN 201610148083A CN 105568243 B CN105568243 B CN 105568243B
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- graphene
- stainless steel
- corrosion
- inhibiting coating
- graphene film
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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
-
- 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 carbon nanomaterial preparation technology field, it is related to a kind of graphene corrosion-inhibiting coating preparation method for stainless steel surface, first using native graphite as raw material, graphene powder is prepared by oxidation-reduction method, then graphene powder be freeze-dried spare, graphene powder is placed in tablet press machine again and is pressed into graphene film, then graphene film is placed on the top of stainless steel base, target of the graphene film as ion sputtering, ion sputtering is carried out to graphene film using energetic ion rifle, the broken surface that stainless steel sample is covered in so as to uniform deposition of graphene film after ion sputtering, graphene corrosion-inhibiting coating is made in stainless steel sample surfaces；The graphene corrosion-inhibiting coating of preparation is uniform, and thickness is easily controllable, and the device used is simple, and preparation efficiency is high, and energy consumption is low, and antiseptic property is superior.
Description
Technical field：
The invention belongs to carbon nanomaterial preparation technology field, is related to a kind of ion sputtering process and prepares graphene corrosion-inhibiting coating
Technique, particularly a kind of graphene corrosion-inhibiting coating preparation method for stainless steel surface, the graphene coating antiseptic of preparation
Excellent performance.
Background technology：
Graphene is a kind of new carbon, has excellent heat conduction and electric conductivity, high transparency, high intensity, also has
The many advantages such as abundant raw material, small toxicity, biocompatibility, lead in pharmaceutical carrier, energy storage, sensor preparation, optics, catalysis etc.
Domain has great application value.Stainless steel has the excellent characteristics such as preferable intensity, higher wearability, therefore extensively should
Various aspects for lives such as pipeline, public utility, highways.Annual China is because of Corrosion of Stainless Steel, and the economy suffered
Loss is up to exceeded 100 billion, therefore becomes a kind of necessary come the antiseptic property of hardened stainless steel to reduce economic loss by coating
Measure.Report at present on hardened stainless steel antiseptic property method is very much, mainly including zinc, chromium, clay-like material cladding
Deng these materials being employed often have certain injury to environment and human body or have water imbibition, it is difficult to realize a wide range of
Application and efficient anti-corrosion.Therefore, a kind of quick, simple, cheap, nontoxic, isolation water and air high efficiency coating system is explored
It is standby to be highly desirable, the advantages such as ion sputtering process has device relative to other methods such as electrochemical process and manufacturing process is simple,
It is that what is grown up in recent years prepare a kind of very important method of high-quality thin film, it has other technologies incomparable
Advantage, in film-forming process, deposition velocity is slow, the thickness of film and quality are easy to control.Therefore, comprehensive grapheme material itself is excellent
The preparation of different antiseptic property and ion sputtering process high-quality thin film, seeks a kind of graphene anti-corrosion for stainless steel surface and applies
Layer preparation method, in the preparation process of coating, graphene sheet layer, which is broken, to diminish, it can be achieved that the dense packing of higher degree,
Stainless steel is set to reach efficient water proof and exhausted gas.
The content of the invention：
It is an object of the invention to overcome the prior art and raw material there are the shortcomings that, seek design and a kind of be used for not be provided
The graphene corrosion-inhibiting coating preparation method for steel surface of becoming rusty, prepares graphene corrosion-inhibiting coating, the stone prepared based on ion sputtering process
Black alkene corrosion-inhibiting coating have the advantages that stablize, efficiently, small toxicity, isolation water and air, can hardened stainless steel antiseptic property.
To achieve these goals, the technique of the invention for preparing graphene corrosion-inhibiting coating specifically includes following steps：
(1), using native graphite as raw material, graphene powder is prepared by oxidation-reduction method, then to Graphene powder
End is freeze-dried, and first will react 12 at 30 degrees Celsius after 0.1g graphite, 0.3g potassium permanganate, and the mixing of the 90ml concentrated sulfuric acids
Hour obtains graphite oxide, will be dissolved in after obtained graphite oxide centrifuge washing in 200ml distilled water, and it is micro- then to add 100
Rise hydrazine hydrate, when 95 degrees Celsius of lower reductase 12s are small after obtained sample centrifuged, be freeze-dried, obtain graphene powder；
(2), graphene powder is placed in tablet press machine, graphene powder is pressed into by graphene film with the pressure of 30Mpa；
(3), graphene film prepared by step (2) is placed on the top of stainless steel base, graphene film be used as from
The target of son sputtering, ion sputtering, the graphene film after ion sputtering are carried out using energetic ion rifle to graphene film
The broken surface that stainless steel sample is covered in so as to uniform deposition, graphene corrosion-inhibiting coating is made in stainless steel sample surfaces,
The accelerating potential of wherein ion sputtering is arranged to 300V, in deposition process the air pressure of argon gas and flow velocity be respectively 0.04Pa and
4cm3/ min, sputtering time are arranged to 1h, 2h, 3h or 5h.
Oxidizing process of the present invention is improved HUMMERS methods, and reduction method is carried out thoroughly also by hydrazine hydrate reduction agent
It is former.
The present invention is characterized as the graphene corrosion-inhibiting coating to obtained by using means of different, and used means include
Scanning electron microscope (SEM), x-ray photoelectron spectroscopy (XPS).
The present invention, with electrochemical methods such as polarization curve and electrochemical impedances, prevents material by electrochemical workstation
Rotten performance is detected, and has the polarization curve forward migration of the sample of graphene corrosion-inhibiting coating, and corrosion current reduces, while electricity
Chemical impedance becomes larger, this shows the raising of antiseptic property, and the corrosion rate of stainless steel is reduced to by 0.019mm/year
0.00138mm/year, reduces 12.76 times.
Compared with prior art, the present invention has the following advantages：First, the graphene corrosion-inhibiting coating prepared is uniform, thickness is easy
It is simple in control, the device used；Second, preparation efficiency is high, the time for completing primary first-order equation is shorter, it is only necessary to 30-60min；Third,
Energy consumption is low, and graphene makes low in raw material price, and ion sputtering energy consumption is low；Fourth, graphene corrosion-inhibiting coating is in stainless steel surface heap
Product is close, and antiseptic property is superior, and corrosion 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%；Fifth, graphene corrosion-inhibiting coating is applied to stainless steel antiseptic property
Strengthen, prepare and stablize, reproducible, efficient, the carbon quantum dot quality of preparation is good, and performance is stablized.
Brief description of the drawings：
Fig. 1 is that the present invention prepares the apparatus structure principle schematic of graphene corrosion-inhibiting coating, including energetic ion rifle,
Graphene film, stainless steel base.
Fig. 2 is that the SEM of graphene corrosion-inhibiting coating prepared by the present invention schemes (D), the SEM of pure stainless steel schemes (A and B) and not
Rust steel surface has corrosion-inhibiting coating and the comparison diagram (C) without corrosion-inhibiting coating.
Fig. 3 is that the XPS of stainless steel sample with graphene corrosion-inhibiting coating prepared by the present invention and pure stainless steel sample schemes.
Fig. 4 is that the embodiment of the present invention has the stainless steel sample of corrosion-inhibiting coating and pure stainless steel sample TAFEL curve maps
(A), corrosion rate figure (B), open-circuit voltage figure (C) and preservative efficiency figure (D).
Embodiment：
The invention will be further described by way of example and in conjunction with the accompanying drawings.
Embodiment 1：
The technique that the present embodiment prepares graphene corrosion-inhibiting coating specifically includes following steps：
(1), using native graphite as raw material, graphene powder is prepared by oxidation-reduction method, then to Graphene powder
End is freeze-dried, and first will react 12 at 30 degrees Celsius after 0.1g graphite, 0.3g potassium permanganate, and the mixing of the 90ml concentrated sulfuric acids
Hour obtains graphite oxide, will be dissolved in after obtained graphite oxide centrifuge washing in 200ml distilled water, and it is micro- then to add 100
Rise hydrazine hydrate, when 95 degrees Celsius of lower reductase 12s are small after obtained sample centrifuged, be freeze-dried, obtain graphene powder；
(2), graphene powder is placed in tablet press machine, graphene powder is pressed into by graphene film with the pressure of 30Mpa；
(3), graphene film prepared by step (2) is placed on the top of stainless steel base, graphene film be used as from
The target of son sputtering, ion sputtering, the graphene film after ion sputtering are carried out using energetic ion rifle to graphene film
The broken surface that stainless steel sample is covered in so as to uniform deposition, graphene corrosion-inhibiting coating is made in stainless steel sample surfaces,
The accelerating potential of wherein ion sputtering is arranged to 300V, in deposition process the air pressure of argon gas and flow velocity be respectively 0.04Pa and
4cm3/min。
The time of the present embodiment control ion sputtering is respectively 2h, 3h and 5h, so as to fulfill the control of corrosion-inhibiting coating thickness,
Experimental result shows, during 3h, corrosion-inhibiting coating thickness is suitable, and anti-corrosion effect reaches optimum efficiency.
Claims (1)
1. a kind of graphene corrosion-inhibiting coating preparation method for stainless steel surface, it is characterised in that specifically include following steps：
(1), using native graphite as raw material, graphene powder is prepared by oxidation-reduction method, then to graphene powder into
Row freeze-drying, first will be 12 small in 30 degrees Celsius of reactions after 0.1g graphite, 0.3g potassium permanganate, and the mixing of the 90mL concentrated sulfuric acids
When obtain graphite oxide, will be dissolved in after obtained graphite oxide centrifuge washing in 200mL distilled water, then add 100 microlitres
Hydrazine hydrate, when 95 degrees Celsius of lower reductase 12s are small after obtained sample centrifuged, be freeze-dried, obtain graphene powder；
(2), graphene powder is placed in tablet press machine, graphene powder is pressed into by graphene film with the pressure of 30MPa；
(3), graphene film prepared by step (2) is placed on to the top of stainless steel base, graphene film is splashed as ion
The target penetrated, carries out ion sputtering, graphene film is beaten after ion sputtering using energetic ion rifle to graphene film
The broken surface that stainless steel sample is covered in so as to uniform deposition, graphene corrosion-inhibiting coating is made in stainless steel sample surfaces, wherein
The accelerating potential of ion sputtering is arranged to 300V, and the air pressure of argon gas and flow velocity are respectively 0.04Pa and 4cm in deposition process3/
Min, sputtering time are arranged to 1h, 2h, 3h or 5h.
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| CN201610148083.8A CN105568243B (en) | 2016-03-16 | 2016-03-16 | A kind of graphene corrosion-inhibiting coating preparation method for stainless steel surface |
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| CN201610148083.8A CN105568243B (en) | 2016-03-16 | 2016-03-16 | A kind of graphene corrosion-inhibiting coating preparation method for stainless steel surface |
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| CN105568243B true CN105568243B (en) | 2018-04-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105908053B (en) * | 2016-05-27 | 2018-02-13 | 天津平高智能电气有限公司 | A kind of graphene stainless steel composite material and its preparation method and application |
| 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 |
| 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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|---|---|---|---|---|
| CN102646518A (en) * | 2012-05-08 | 2012-08-22 | 同济大学 | Method for fabricating graphene electrode materials through pulsed laser deposition and application thereof |
| CN102897750A (en) * | 2011-07-29 | 2013-01-30 | 浙江大学 | PrPrearation method for graphene film |
| CN103469203A (en) * | 2013-08-30 | 2013-12-25 | 中国科学院过程工程研究所 | Base material for coating two-dimensional atomic crystals, and continuous production line and method thereof |
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| US5080455A (en) * | 1988-05-17 | 1992-01-14 | William James King | Ion beam sputter processing |
| KR101403989B1 (en) * | 2010-11-09 | 2014-06-10 | 포항공과대학교 산학협력단 | Graphene coated steel and method for preparing thereof |
| CN102557013B (en) * | 2010-12-28 | 2013-10-30 | 国家纳米科学中心 | Preparation method for reduced graphene oxide |
| CN102120574A (en) * | 2011-03-15 | 2011-07-13 | 东南大学 | Method for preparing large-scale two-dimensional nanomaterial graphite |
| CN102275906B (en) * | 2011-06-09 | 2012-12-26 | 西安工业大学 | Method for preparing graphene at normal temperature |
| CN104505262B (en) * | 2014-12-12 | 2017-06-20 | 盐城市新能源化学储能与动力电源研究中心 | A kind of Graphene lead composite material and the Graphene lead carbon electrode prepared using the material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102897750A (en) * | 2011-07-29 | 2013-01-30 | 浙江大学 | PrPrearation method for graphene film |
| CN102646518A (en) * | 2012-05-08 | 2012-08-22 | 同济大学 | Method for fabricating graphene electrode materials through pulsed laser deposition and application thereof |
| CN103469203A (en) * | 2013-08-30 | 2013-12-25 | 中国科学院过程工程研究所 | Base material for coating two-dimensional atomic crystals, and continuous production line and method thereof |
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Effective date of registration: 20210401 Address after: 457000 jiangfengyuan community, Daqing Road, Puyang City, Henan Province Patentee after: PUYANG SHUNKANG PETROLEUM ENGINEERING TECHNOLOGY Co.,Ltd. Address before: 221000 Shimao Square Inner Commercial Street 2, Office 1, Office 2, Building 1-910, Yunlong District, Xuzhou City, Jiangsu Province Patentee before: Jiangsu Shifeng Enterprise Management Consulting Co.,Ltd. |
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