CN109055910A - Integrated (Cr, Cu)-GLC composite coating of a kind of wear-and corrosion-resistant anti-pollution and preparation method thereof - Google Patents
Integrated (Cr, Cu)-GLC composite coating of a kind of wear-and corrosion-resistant anti-pollution and preparation method thereof Download PDFInfo
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- CN109055910A CN109055910A CN201811155221.0A CN201811155221A CN109055910A CN 109055910 A CN109055910 A CN 109055910A CN 201811155221 A CN201811155221 A CN 201811155221A CN 109055910 A CN109055910 A CN 109055910A
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
-
- 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 present invention relates to a kind of wear-and corrosion-resistant anti-pollution integration (Cr, Cu)-GLC composite coating, the composite coating refers to based on atomic percentage, in GLC coated substrate comprising element Cr 3 ~ 10 at.%, Cu 5 ~ 20 at.%, C 70 ~ 90 at.% carbon-based composite coating.Meanwhile the invention also discloses the preparation methods of the composite coating.Inside solid of the present invention, surface is smooth, adhesive force is strong, has excellent tribology performance under marine environment, while having both good anti-corrosion and antifouling property, can be applied to the fields such as petrochemical industry, ocean engineering, ship machinery.
Description
Technical field
The present invention relates in marine environment mechanical movement surfacecti proteon field more particularly to a kind of wear-and corrosion-resistant anti-pollution one
Body (Cr, Cu)-GLC composite coating and preparation method thereof.
Background technique
21 century, strategic position of the ocean in the whole world become increasingly conspicuous, as what China ocean was explored deepens continuously, underwater machine
The surfacecti proteon problem of tool moving component is gradually concerned by people and payes attention to.Under marine environmental conditions, mechanical movement portion
Part will not only bear the damage of fretting wear bring, while further suffer from corrosion and pollution from seawater and marine organisms etc.,
It thus wears more serious.
Currently, offshore equipment is with surface protection coating, often function is relatively simple, is broadly divided into and increases surface abrasion resistance
PVD hard coat and organotin, cuprous oxide, organosilicon and the Organic fluoride and the modified resin that improve surface antifouling property etc. are antifouling
Coating.PVD coating often hardness and wearability with higher, but its ability for not having antibiont attachment, certain oceans are raw
Object can increase the resistance of motion of underwater component in its surface raised growth, breeding, seriously affect the movement effect of mechanical part
Rate and stability.And although organic antifouling paint anti-pollution antiseptic property is excellent, the performance of its friction and wear behavior is general, is easy mill
Loss effect.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of wear-and corrosion-resistant anti-pollution of good performance integration (Cr,
Cu)-GLC composite coating.
Another technical problem to be solved by this invention is to provide the wear-and corrosion-resistant anti-pollution integration (Cr, Cu)-GLC
The preparation method of composite coating.
To solve the above problems, a kind of wear-and corrosion-resistant anti-pollution integration compound painting of (Cr, Cu)-GLC of the present invention
Layer, it is characterised in that: the composite coating refers to based on atomic percentage, includes 3 ~ 10 at. of element Cr in GLC coated substrate
5 ~ 20 at. % of %, Cu, the carbon-based composite coating of 70 C ~ 90 at. %.
Minimum coefficient of friction of the composite coating under briny environment is 0.08.
A kind of preparation method of integrated (Cr, Cu)-GLC composite coating of wear-and corrosion-resistant anti-pollution as described above, including with
Lower step:
(1) substrate is cleaned:
It is cleaned by ultrasonic each 10 min of bloom exemplar respectively with dehydrated alcohol and acetone soln, then with being dried with nitrogen, it then will be described
Exemplar is put into vacuum chamber and is vacuumized；
(2) substrate surface pre-sputter cleaning:
When vacuum degree is better than 3 × 10-3When Pa, it is passed through argon gas at room temperature, control internal vacuum chamber pressure is 0.5 ~ 3 Pa, in institute
It states and adds pulsed bias power supply on exemplar, the exemplar is carried out in advance with argon plasma under conditions of -400 ~ -800 V
5 ~ 60 min of sputter clean；
(3) coating deposits:
After the argon plasma cleaning, adjusting ar pressure is 1 ~ 5 Pa, and adjustment bias is -30 ~ -150 V, on Cr target
Add DC power supply, adjust electric current to deposit 2 ~ 10 min under conditions of 3 ~ 5A to get Cr transition zone；
After the completion of the Cr transition zone deposition, adjusting ar pressure is 1 ~ 5 Pa, adjusts bias -30 ~ -150 V, adjusts Cr target
Electric current be 3 ~ 5A, adjustings Cu target current be 0.5 ~ 2 A, adjustings graphite target current be 2 ~ 5 A, through 1 ~ 6 h deposit to obtain the final product (Cr,
Cu) multi-element doping GLC coating.
Compared with the prior art, the present invention has the following advantages:
1, the present invention uses multi-element doping magnetron sputtering technology, functional doped chemical Cr and Cu is chosen, by adjusting plating
Membrane process parameter optimizes doping content, so that obtaining has excellent tribology performance under marine environment, while having both good
Anti-corrosion and the inside solid of antifouling property, the multifunctional C base composite coating that surface is smooth, adhesive force is strong.
2, present invention addition of Cr element in GLC coated substrate can play the role of raising coating hardness, corrosion proof.
3, coefficient of friction minimum of (Cr, the Cu)-GLC multicomponent composite coating that the present invention obtains under briny environment rubs
Wiping coefficient realizes 0.08 compared with low friction, and the duration is longer.Simultaneously in friction process, the open-circuit voltage of coating
Also higher, show higher corrosion resistance.
4, in (Cr, Cu)-GLC multicomponent composite coating that the present invention obtains, since the addition of Cu element can be in seawater ring
Bacterium is killed under border and therefore aufwuch so that its anti-seaweed adhesion property under briny environment is excellent, embodies excellent
Antifouling property.
5, the composite coating deposition rate that the present invention obtains is very fast, and even film layer, compact structure, internal stress is small, and hardness is 5
~ 17 GPa or so, the contact angle between coating and seawater have certain hydrophobicity between 86 ~ 96 °.
6, the preparation of composite coating of the present invention is implemented at room temperature, and substrate is not necessarily to any additional heating process, prepared
Composite coating have a good application prospect in fields such as petrochemical industry, ocean engineering, ship machineries.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 is the section SEM picture of (Cr, Cu)-GLC multi-element coating prepared by the present invention.
The schematic diagram for the electrochemistry friction and wear test that Fig. 2 is implemented for the present invention.
Fig. 3 is the electrochemistry friction and wear test result of the embodiment of the present invention 1 and comparative example 1.
Fig. 4 is the angle of wetting result of coating and artificial seawater prepared by the embodiment of the present invention 1.
Fig. 5 is that the embodiment of the present invention 2 and 2 seaweed of comparative example adhere to experimental results.
Specific embodiment
A kind of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution of embodiment 1, the composite coating refer to by original
Sub- percentage meter, the carbon in GLC coated substrate comprising 4.3 at. % of element Cr, 12.5 Cu at. %, 83.2 C at. %
Base composite coating.
The preparation method of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution, comprising the following steps:
(1) substrate is cleaned:
It is cleaned by ultrasonic each 10 min of bloom exemplar respectively with dehydrated alcohol and acetone soln, then with being dried with nitrogen, then by exemplar
It is put into vacuum chamber and is vacuumized；
(2) substrate surface pre-sputter cleaning:
When vacuum degree is better than 3 × 10-3It can start plated film work when Pa, be passed through argon gas at room temperature, control internal vacuum chamber pressure
By force it is 0.5 Pa, pulsed bias power supply is added on exemplar, exemplar is carried out in advance with argon plasma under conditions of -400 V
60 min of sputter clean, with remove surface oxide layer and other impurity；
(3) coating deposits:
Argon plasma cleaning after, adjustings ar pressure be 1 Pa, adjustment bias be -30 V, on Cr target add DC power supply,
It adjusts under conditions of electric current is 3 A and deposits 10 min to get Cr transition zone；
After the completion of Cr transition zone deposition, adjusting ar pressure is 1 Pa, adjusts -150 V of bias, and adjusting Cr target current is 3 A,
Adjusting Cu target current is 0.5 A, and adjusting graphite target current is 3.5 A, deposits through 6 h and applies up to (Cr, Cu) multi-element doping GLC
Layer.
The section SEM picture of prepared (Cr, Cu) multi-element doping GLC coating is as shown in Figure 1, the thickness of coating is about
2.5 μm。
A kind of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution of embodiment 2, the composite coating refer to by original
Sub- percentage meter, in GLC coated substrate comprising 10 at. % of element Cr, 20 Cu at. %, 70 C at. % it is carbon-based multiple
Close coating.
The preparation method of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution, comprising the following steps:
(1) substrate is cleaned:
It is cleaned by ultrasonic each 10 min of bloom exemplar respectively with dehydrated alcohol and acetone soln, then with being dried with nitrogen, then by exemplar
It is put into vacuum chamber and is vacuumized；
(2) substrate surface pre-sputter cleaning:
When vacuum degree is better than 3 × 10-3It can start plated film work when Pa, be passed through argon gas at room temperature, control internal vacuum chamber pressure
By force it is 3 Pa, pulsed bias power supply is added on exemplar, exemplar is splashed in advance with argon plasma under conditions of -800 V
Penetrate cleaning 5 min, with remove surface oxide layer and other impurity；
(3) coating deposits:
After argon plasma cleaning, adjusting ar pressure is 5 Pa, and adjustment bias is -150 V, and direct current is added on Cr target
Source adjusts electric current to deposit 2 min under conditions of 5A to get Cr transition zone；
After the completion of Cr transition zone deposition, adjusting ar pressure is 5 Pa, adjusts -30 V of bias, and adjusting Cr target current is 5A, is adjusted
Cu target current is 2 A, and adjusting graphite target current is 5 A, is deposited through 1 h up to (Cr, Cu) multi-element doping GLC coating.
A kind of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution of embodiment 3, the composite coating refer to by original
Sub- percentage meter, in GLC coated substrate comprising 3 at. % of element Cr, 7 Cu at. %, 90 C at. % it is carbon-based compound
Coating.
The preparation method of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution, comprising the following steps:
(1) substrate is cleaned:
It is cleaned by ultrasonic each 10 min of bloom exemplar respectively with dehydrated alcohol and acetone soln, then with being dried with nitrogen, then by exemplar
It is put into vacuum chamber and is vacuumized；
(2) substrate surface pre-sputter cleaning:
When vacuum degree is better than 3 × 10-3It can start plated film work when Pa, be passed through argon gas at room temperature, control internal vacuum chamber pressure
By force it is 3 Pa, pulsed bias power supply is added on exemplar, exemplar is splashed in advance with argon plasma under conditions of -800 V
Penetrate cleaning 5 min, with remove surface oxide layer and other impurity；
(3) coating deposits:
After argon plasma cleaning, adjusting ar pressure is 5 Pa, and adjustment bias is -150 V, and direct current is added on Cr target
Source adjusts electric current to deposit 2 min under conditions of 5A to get Cr transition zone；
After the completion of Cr transition zone deposition, adjusting ar pressure is 5 Pa, adjusts -30 V of bias, and adjusting Cr target current is 3 A, is adjusted
Section Cu target current is 0.5 A, and adjusting graphite target current is 5 A, is deposited through 5 h up to (Cr, Cu) multi-element doping GLC coating.
A kind of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution of embodiment 4, the composite coating refer to by original
Sub- percentage meter, the carbon in GLC coated substrate comprising 9.8 at. % of element Cr, 5.0 Cu at. %, 85.2 C at. %
Base composite coating.
The preparation method of integrated (Cr, the Cu)-GLC composite coating of the wear-and corrosion-resistant anti-pollution, comprising the following steps:
(1) substrate is cleaned:
It is cleaned by ultrasonic each 10 min of bloom exemplar respectively with dehydrated alcohol and acetone soln, then with being dried with nitrogen, then by exemplar
It is put into vacuum chamber and is vacuumized；
(2) substrate surface pre-sputter cleaning:
When vacuum degree is better than 3 × 10-3It can start plated film work when Pa, be passed through argon gas at room temperature, control internal vacuum chamber pressure
By force it is 1 Pa, pulsed bias power supply is added on exemplar, exemplar is splashed in advance with argon plasma under conditions of -600 V
Penetrate cleaning 30 min, with remove surface oxide layer and other impurity；
(3) coating deposits:
Argon plasma cleaning after, adjustings ar pressure be 2 Pa, adjustment bias be -60 V, on Cr target add DC power supply,
It adjusts under conditions of electric current is 4A and deposits 5 min to get Cr transition zone；
After the completion of Cr transition zone deposition, adjusting ar pressure is 3 Pa, adjusts -90 V of bias, and adjusting Cr target current is 4 A, is adjusted
Section Cu target current is 1.5 A, and adjusting graphite target current is 2 A, deposits through 4.5 h and applies up to (Cr, Cu) multi-element doping GLC
Layer.
Minimum coefficient of friction of the composite coating under briny environment in above-described embodiment 1 ~ 4 is 0.08.
Comparative example 1:
The 9Cr18 bloom of the standard analysis of domestic certain producer production, surface free coating treatment；
Comparative example 2:
The 9Cr18 bloom of the standard analysis of domestic certain producer production, the wear-resisting type GLC that surface coats the production of certain Coatings Corporation are applied
Layer.
[electrochemistry frictional wear experiment]
Using MFT-R4000 electrochemistry friction wear testing machine, to a series of (Cr, Cu) multi-element doping prepared by embodiment 1
The electrochemistry friction and abrasion of non-coating 9Cr18 steel in GLC coating and comparative example 1 can be carried out test.The mechanism figure of test is such as
Shown in Fig. 2, sample is contacted and is back and forth rubbed with mating material (alumina balls that diameter is 6.0 mm) in artificial seawater medium
It wipes, loading force is 10 N, 0.1 Hz of frequency, and electrochemistry-friction curve is shown in Fig. 3, it is seen that coating sample prepared by the present invention
Average friction coefficient it is lower, minimum coefficient of friction be 0.08, the coefficient of friction than the bloom sample of comparative example 1 reduces about 4
Times.Meanwhile coating prepared by the present invention possesses higher open-circuit voltage, about+0.00 V in friction, it means that coating exists
Corrosion resistance in seawater is good.
[wetability experiment]
Using OCA20 contact angle measurement to (Cr, Cu) multi-element doping GLC coating prepared in embodiment 1 and artificial sea
Contact angle between water measures, as a result as shown in Figure 4, it is seen that the contact angle of coating is about 92 °, it is shown that certain is hydrophobic
Property.
[seaweed attachment experiment]
To business in (Cr, Cu) multi-element doping GLC coating and comparative example 2 for preparing in embodiment 2 of the present invention
Change GLC coating and carried out seaweed adhesion comparative experiments, as a result as shown in Figure 5.Each bright spot represents Du of attachment in figure
Family name seaweed, it is seen that compared to business GLC coating (Fig. 5 a), (Cr, Cu) multi-element doping GLC prepared by the embodiment of the present invention 2 is applied
The seaweed adhesion amount of layer surface is substantially reduced, and has excellent antifouling property.
Claims (3)
1. a kind of integrated (Cr, the Cu)-GLC composite coating of wear-and corrosion-resistant anti-pollution, it is characterised in that: the composite coating refer to by
Atomic percentage meter includes 3 ~ 10 at. % of element Cr, 5 Cu ~ 20 at. %, 70 C ~ 90 at. % in GLC coated substrate
Carbon-based composite coating.
2. integrated (Cr, Cu)-GLC composite coating of a kind of wear-and corrosion-resistant anti-pollution as described in claim 1, it is characterised in that:
Minimum coefficient of friction of the composite coating under briny environment is 0.08.
3. a kind of preparation method of integrated (Cr, Cu)-GLC composite coating of wear-and corrosion-resistant anti-pollution as described in claim 1,
The following steps are included:
(1) substrate is cleaned:
It is cleaned by ultrasonic each 10 min of bloom exemplar respectively with dehydrated alcohol and acetone soln, then with being dried with nitrogen, it then will be described
Exemplar is put into vacuum chamber and is vacuumized；
(2) substrate surface pre-sputter cleaning:
When vacuum degree is better than 3 × 10-3When Pa, it is passed through argon gas at room temperature, control internal vacuum chamber pressure is 0.5 ~ 3 Pa, in institute
It states and adds pulsed bias power supply on exemplar, the exemplar is carried out in advance with argon plasma under conditions of -400 ~ -800 V
5 ~ 60 min of sputter clean；
(3) coating deposits:
After the argon plasma cleaning, adjusting ar pressure is 1 ~ 5 Pa, and adjustment bias is -30 ~ -150 V, on Cr target
Add DC power supply, adjust electric current to deposit 2 ~ 10 min under conditions of 3 ~ 5A to get Cr transition zone；
After the completion of the Cr transition zone deposition, adjusting ar pressure is 1 ~ 5 Pa, adjusts bias -30 ~ -150 V, adjusts Cr target
Electric current be 3 ~ 5A, adjustings Cu target current be 0.5 ~ 2 A, adjustings graphite target current be 2 ~ 5 A, through 1 ~ 6 h deposit to obtain the final product (Cr,
Cu) multi-element doping GLC coating.
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|---|---|---|---|
| CN201811155221.0A CN109055910B (en) | 2018-09-30 | 2018-09-30 | Wear-resistant, corrosion-resistant and anti-fouling integrated (Cr, Cu) -GLC composite coating and preparation method thereof |
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|---|---|---|---|
| CN201811155221.0A CN109055910B (en) | 2018-09-30 | 2018-09-30 | Wear-resistant, corrosion-resistant and anti-fouling integrated (Cr, Cu) -GLC composite coating and preparation method thereof |
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| CN109055910B CN109055910B (en) | 2020-10-02 |
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| CN110643943A (en) * | 2019-10-15 | 2020-01-03 | 河南科技大学 | Graphite-like carbon doped film, preparation method thereof and workpiece |
| WO2022242732A1 (en) * | 2021-05-21 | 2022-11-24 | 华为技术有限公司 | Ecg electrode and preparation method therefor, and electronic device |
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| Publication number | Publication date |
|---|---|
| CN109055910B (en) | 2020-10-02 |
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