CN109112604A - A kind of graphene oxide/cobalt-based composite deposite and its preparation method and application - Google Patents
A kind of graphene oxide/cobalt-based composite deposite and its preparation method and application Download PDFInfo
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- CN109112604A CN109112604A CN201810940002.7A CN201810940002A CN109112604A CN 109112604 A CN109112604 A CN 109112604A CN 201810940002 A CN201810940002 A CN 201810940002A CN 109112604 A CN109112604 A CN 109112604A
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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
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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Abstract
The invention discloses a kind of graphene oxide/cobalt-based composite deposites and its preparation method and application, the composite deposite is using cobalt, nickel or cobalt-nickel alloy as anode, workpiece to be plated is cathode, in anode and cathode immersion composite plating solution after ultrasonic vibration, electro-deposition will be carried out on workpiece to be plated using pulse current and is made；It is counted according to deionized water and each substance total volume 1L, the composite plating solution includes 30~200g/L of cobalt salt, 30~200g/L of nickel salt, 5~80g/L of phosphate, 10~60g/L of boric acid, 10~50g/L of complexing agent, 0.1~5g/L of graphene oxide.Preparation method of the present invention is simple, efficient and environmentally protective.The composite deposite has high rigidity, excellent antiwear and antifriction and corrosion resistance.It can be used as function protecting layer and be widely used in various requirement high rigidity, high abrasion, low-friction coefficient and corrosion resistant component of machine.
Description
Technical field
The invention belongs to function of surface thin-film material technical fields, multiple more particularly, to a kind of graphene oxide/cobalt-based
Close coating and its preparation method and application.
Background technique
Metal material is now using most engineering material, and abrasion, corrosion and the fracture failure of metal parts are to warp
Ji brings huge loss.In fact, the failure of metal material mainly starts from its surface, as long as by surface engineering technology at it
Surface obtains certain thickness function protecting layer, it will be able to effectively improve the comprehensive performance of metal material and extend it and be on active service the longevity
Life.Electro-deposition techniques are due to having many advantages, such as easy to operate, economical and efficient and coating microscopic appearance is easy to control and is answered extensively
Coating material for metal parts surface deposition high rigidity, the wear-resistant performances such as anti-corrosion, heat-resisting and beauty.Past, hard chrome
(Cr) coating is widely used in the protective layer of metal parts since high with hardness, Wear resistance and Anti corrosion energy is beautiful.But from environment
Angle considers that electrodeposited chromium seriously pollutes environment, endangers health, and countries in the world government has all formulated the policy and method of some classes
Rule are limited and are forbidden to sexavalence Cr product.In terms of the hard Cr coating of alternate functionality, nickel-phosphor (Ni-P) coating is due to performance
The excellent concern for causing many scholars.However, nickel is face-centered cubic lattice, easily occur with antithesis metal in friction process serious
Adhesion, the coefficient of friction of Ni-P coating is higher, and wearability is to be improved.Cobalt (Co) is close-packed hexagonal lattice, in friction process
It is avoided that and adheres with antithesis metal, Co is added in Ni-P coating, preparation Co-Ni-P coating is expected to show more excellent
Different antiwear and friction reduction property.In addition, graphene oxide (GO) is due to the performance excellent with graphene, such as self-lubricating, high intensity
Deng, also have oxygen-containing functional group abundant (hydroxyl, carboxyl etc.) make it have preferable water solubility.GO is embedded into Co-Ni-P
It is expected to further increase hardness, antiwear and antifriction and the corrosion resisting property of composite deposite in coating.However, at present both at home and abroad about cobalt-based
Composite deposite, especially antiwear and antifriction and corrosion-resistant integrated oxidization graphite/cobalt-based composite deposite, also seldom see related patents
It is reported with paper.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, it is an object of that present invention to provide a kind of graphite oxides
Alkene/cobalt-based composite deposite.Not only hardness is high for graphene oxide prepared by the present invention/cobalt-based composite deposite, but also has excellent
Antiwear and antifriction and corrosion resistance.
Another object of the present invention is to provide above-mentioned graphene oxide/cobalt-based composite deposite preparation method.This method letter
It is single, economical and environmentally protective.
Still a further object of the present invention is to provide the application of above-mentioned graphene oxide/cobalt-based composite deposite.
The purpose of the present invention is realized by following technical proposals:
A kind of graphene oxide/cobalt-based composite deposite, the graphene oxide/cobalt-based composite deposite are with cobalt, nickel or cobalt-
Nickel alloy is anode, and workpiece to be plated is cathode, sets two interelectrode distances, and above-mentioned anode and cathode is immersed in composite plating solution
After ultrasonic vibration, electro-deposition is carried out on workpiece to be plated using pulse current and is made, it is overall according to deionized water and each substance
Product 1L meter, the composite plating solution includes 30~200g/L of cobalt salt, 30~200g/L of nickel salt, 5~80g/L of phosphate, boric acid 10
~60g/L, 10~50g/L of complexing agent, 0.1~5g/L of graphene oxide.
Preferably, the graphene oxide is to be prepared using Hummers method, and two dimension is having a size of 0.1~5 μm, with a thickness of 1
~20 atomic layers.
Preferably, the time of the ultrasound is 10~30min, and the power of the ultrasound is 50~100W.
Preferably, the cobalt salt is cobaltous sulfate or/and cobalt chloride, and the nickel salt is nickel sulfate or/and nickel chloride, the phosphorus
Hydrochlorate is sodium hypophosphite or/and sodium phosphate；The complexing agent is sodium citrate, sodium gluconate, ammonium citrate or EDETATE SODIUM
One or more of.
Preferably, the pH value of the composite plating solution is 2~6.
Preferably, two interelectrode distance is 1~5cm, and the time of the electro-deposition is 30~80min.
Preferably, the parameter of the electro-deposition are as follows: magnetic stirring speed is 200~600rpm, and the temperature of electro-deposition is 20
~80 DEG C, average current density is 0.2~2A/dm2, duty ratio is 20~50%, and frequency is 200~1000Hz.
Preferably, the workpiece to be plated is copper, steel, titanium or its alloy, and the surface roughness of the workpiece to be plated is 0.06
~0.1 μm.
The graphene oxide/cobalt-based composite deposite preparation method, comprises the following specific steps that:
S1. configure composite plating solution: by cobalt salt, nickel salt, phosphate, boric acid, complexing agent, graphene oxide be dissolved in from
It is 2~6 with the pH value that sodium hydroxide and dilute sulfuric acid adjust electroplate liquid in sub- water；
S2. anode is cobalt, nickel or cobalt-nickel alloy, and cathode is workpiece to be plated, sets two interelectrode distances as 1~5cm, incites somebody to action
Above-mentioned anode and cathode immerses in composite plating solution obtained by step S1, the ultrasound shake in the ultrasonic vibrator that power is 50~100W
After dynamic 10~30min, electro-deposition is carried out using pulse current, graphene oxide/cobalt-based composite deposite is made on workpiece to be plated.
The graphene oxide/cobalt-based composite deposite answering in automobile, machinery, precision manufactureing and field of aerospace
With.
Compared with prior art, the invention has the following advantages:
1. in graphene oxide prepared by the present invention/cobalt-based composite deposite, graphene oxide in composite deposite uniformly,
It is firmly bonded in the coat of metal, binding force is good between composite deposite and workpiece.
2. graphene oxide prepared by the present invention/cobalt-based composite deposite has both high rigidity, antiwear and antifriction and corrosion resistant
Advantage.During composite deposite and mating material fretting wear, graphene oxide has in the secondary surface and interface formation of friction
Height combines and the continuous transfer membrane of self-lubricating property, can effectively prevent the direct contact of surface of friction pair, to reduce Composite Coatings
The coefficient of friction and wear rate of layer.Graphene oxide, which is filled into composite deposite, can play the role of physical isolation, simultaneous oxidation stone
Black alkene itself has excellent antiseptic property, guarantees composite deposite to etchant gas and liquid barrier, to improve composite deposite
Corrosion resistance.
3. simple easy, the operating procedure stabilization of preparation method of the invention, good economy performance, cost of investment are low, high-efficient and green
Colour circle is protected, it is easy to accomplish industrialized production.It can be in the metal bases such as all size and different copper, steel, titanium or its alloy
Surface prepares graphene oxide/cobalt-based composite deposite.
Replace pollution environment 4. graphene oxide prepared by the present invention/cobalt-based composite deposite has, endanger human body
The hard chromium of health.Suitable for requiring high rigidity, high abrasion, low friction and corrosion resistant component of machine, in automobile, machine
Tool, precision manufactureing and aerospace field have a wide range of applications, and can extend the service life of part, reduce power consumption,
It is energy saving.With good application value and economical, societal benefits.
Detailed description of the invention
Fig. 1 is graphene oxide TEM photo produced by the present invention.
Fig. 2 is graphene oxide/cobalt-based composite deposite SEM photograph made from embodiment 2.
Fig. 3 is graphene oxide/cobalt-based composite deposite average friction coefficient and wear rate made from embodiment 2.
Fig. 4 is graphene oxide/cobalt-based composite deposite corrosion rate made from embodiment 2.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except especially saying
Bright, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Graphene oxide described in Examples 1 to 4 is made using Hummers method, and two dimension is thick having a size of 0.1~5 μm
Degree is 1~20 atomic layer.Fig. 1 is using graphene oxide TEM photo made from Hummers method.
Embodiment 1
1. configuring composite plating solution: by cobaltous sulfate, nickel sulfate, sodium hypophosphite, boric acid, sodium gluconate, graphene oxide
It is dissolved into deionized water, composite plating solution is made；Wherein, the concentration of cobaltous sulfate be 20g/L, the concentration of nickel sulfate be 20g/L,
The concentration of sodium hypophosphite is 16g/L, the concentration of boric acid is 16g/L, the concentration of sodium gluconate is 16g/L, graphene oxide
Concentration is 0.1g/L, is 3 with the pH value that sodium hydroxide and dilute sulfuric acid adjust electroplate liquid.
2. using anode as cobalt piece, cathode is by oil removing-cleaning-acid activation brass base, and distance is between two electrodes
3cm immerses above-mentioned anode and cathode in electroplate liquid obtained by step S1, shakes 20min in the ultrasonic vibrator that power is 50W
Electro-deposition is carried out using pulse current afterwards, graphene oxide/cobalt-based composite deposite is made on brass base.Electro-deposition it is specific
Parameter are as follows: average current density 1.0A/dm2, duty ratio 20%, frequency 500Hz, magnetic stirring speed 300rpm, temperature
Degree is 50 DEG C, time 30min.
Embodiment 2
1. configuring composite plating solution: cobaltous sulfate, nickel sulfate, sodium hypophosphite, boric acid, sodium citrate, graphene oxide is molten
Composite plating solution is made into deionized water in solution；Wherein, the concentration of cobaltous sulfate is 50g/L, the concentration of nickel sulfate is 50g/L, secondary
The concentration of sodium phosphate is 10g/L, the concentration of boric acid is 40g/L, the concentration of sodium citrate is 40g/L, the concentration of graphene oxide
It is 3 with the pH value that sodium hydroxide and dilute sulfuric acid adjust electroplate liquid for 0.2g/L.
2. anode is nickel sheet, cathode is by oil removing-steel matrix of cleaning-acid activation 45, and distance is between two electrodes
2cm immerses above-mentioned anode and cathode in electroplate liquid obtained by step S1, the ultrasonic vibration in the ultrasonic vibrator that power is 100W
Electro-deposition is carried out using pulse current after 30min, graphene oxide/cobalt-based composite deposite is made in No. 45 steel matrix.Electricity is heavy
Long-pending design parameter are as follows: average current density 2.0A/dm2, duty ratio 20%, frequency 1000Hz, magnetic stirring speed is
400rpm, temperature are 45 DEG C, time 70min.
Fig. 2 is graphene oxide/cobalt-based composite deposite surface SEM photograph obtained by the present embodiment.As can be seen from Figure 2, oxygen
Graphite alkene is uniformly distributed and is firmly bound in cobalt-based composite deposite.Fig. 3 and Fig. 4 is respectively that graphene oxide/cobalt-based is compound
Coating (Co-Ni-P-GO), No. 45 steel matrix (45#) and co-based alloy coating (Co-Ni-P) average friction coefficient, wear rate
With comparison between corrosion figure.Wherein, co-based alloy coating (Co-Ni-P) and graphene oxide/cobalt-based composite deposite (Co-Ni-P-
It GO is) with Tongfang method preparation gained.It can be seen that from Fig. 3 and Fig. 4, graphene oxide/cobalt-based composite deposite obtained by the present embodiment
Average friction coefficient and wear rate be respectively 0.29 and 5.29 × 10-6mm3(N.m)-1, corrosion rate is 3.54 × 10-2
(mm·y-1), it is far below No. 45 steel and co-based alloy coating.The result shows that graphene oxide/cobalt-based prepared by the present invention is multiple
It closes coating and has both good antiwear and antifriction and anticorrosion effect simultaneously.
Embodiment 3
1. configuring composite plating solution: cobaltous sulfate, nickel chloride, sodium phosphate, boric acid, ammonium citrate, graphene oxide are dissolved
Into deionized water, composite plating solution is made；Wherein, the concentration of cobaltous sulfate is 100g/L, the concentration of nickel chloride is 100g/L, phosphorus
The concentration of sour sodium is 20g/L, the concentration of boric acid is 30g/L, the concentration of ammonium citrate is 30g/L, the concentration of graphene oxide is
0.5g/L is 4 with the pH value that sodium hydroxide and dilute sulfuric acid adjust electroplate liquid.
2. anode is nickel sheet, cathode is by oil removing-steel matrix of cleaning-acid activation 45, and distance is between two electrodes
4cm immerses above-mentioned anode and cathode in electroplate liquid obtained by step S1, the ultrasonic vibration in the ultrasonic vibrator that power is 80W
Electro-deposition is carried out using pulse current after 30min, graphene oxide/cobalt-based composite deposite is made in No. 45 steel matrix.Electricity is heavy
Long-pending design parameter are as follows: average current density 0.5A/dm2, duty ratio 30%, frequency 1000Hz, magnetic stirring speed is
500rpm, temperature are 50 DEG C, time 60min.
Embodiment 4
1. configuring composite plating solution: cobaltous sulfate, nickel sulfate, sodium hypophosphite, boric acid, sodium citrate, graphene oxide is molten
Composite plating solution is made into deionized water in solution；Wherein, the concentration of cobaltous sulfate is 80g/L, the concentration of nickel sulfate is 80g/L, secondary
The concentration of sodium phosphate is 20g/L, the concentration of boric acid is 40g/L, the concentration of sodium citrate is 40g/L, the concentration of graphene oxide
It is 3 with the pH value that sodium hydroxide and dilute sulfuric acid adjust electroplate liquid for 0.6g/L.
2. anode is cobalt piece, cathode is by oil removing-cleaning-acid activation brass base, and distance is between two electrodes
2cm immerses above-mentioned anode and cathode in electroplate liquid obtained by step S1, the ultrasonic vibration in the ultrasonic vibrator that power is 100W
Electro-deposition is carried out using pulse current after 20min, graphene oxide/cobalt-based composite deposite is made on brass base.Electro-deposition
Design parameter are as follows: average current density 1.5A/dm2, duty ratio 20%, frequency 1000Hz, magnetic stirring speed is
500rpm, temperature are 45 DEG C, time 30min.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of graphene oxide/cobalt-based composite deposite, which is characterized in that the graphene oxide/cobalt-based composite deposite be with
Cobalt, nickel or cobalt-nickel alloy are anode, and workpiece to be plated is cathode, sets two interelectrode distances, above-mentioned anode and cathode are immersed multiple
In conjunction electroplate liquid after ultrasonic vibration, electro-deposition is carried out on workpiece to be plated using pulse current and is made；According to deionized water and
Each substance total volume 1L meter, the composite plating solution include 30~200g/L of cobalt salt, 30~200g/L of nickel salt, and phosphate 5~
80g/L, 10~60g/L of boric acid, 10~50g/L of complexing agent, 0.1~5g/L of graphene oxide.
2. graphene oxide according to claim 1/cobalt-based composite deposite, which is characterized in that the graphene oxide is
It is prepared using Hummers method, two dimension is having a size of 0.1~5 μm, with a thickness of 1~20 atomic layer.
3. graphene oxide according to claim 1/cobalt-based composite deposite, which is characterized in that the time of the ultrasound is
10~30min, the power of the ultrasound are 50~100W.
4. graphene oxide according to claim 1/cobalt-based composite deposite, which is characterized in that the cobalt salt is cobaltous sulfate
Or/and cobalt chloride, the nickel salt are nickel sulfate or/and nickel chloride, the phosphate is sodium hypophosphite or/and sodium phosphate；It is described
Complexing agent is one or more of sodium citrate, sodium gluconate, ammonium citrate or EDETATE SODIUM.
5. graphene oxide according to claim 1/cobalt-based composite deposite, which is characterized in that the composite plating solution
PH value is 2~6.
6. graphene oxide according to claim 1/cobalt-based composite deposite, which is characterized in that two interelectrode distance
For 1~5cm, the time of the electro-deposition is 30~80min.
7. graphene oxide according to claim 1/cobalt-based composite deposite, which is characterized in that the parameter of the electro-deposition
Are as follows: magnetic stirring speed is 200~600rpm, and the temperature of electro-deposition is 20~80 DEG C, and average current density is 0.2~2A/
dm2, duty ratio is 20~50%, and frequency is 200~1000Hz.
8. graphene oxide according to claim 1/cobalt-based composite deposite, which is characterized in that the workpiece to be plated be copper,
Steel, titanium or its alloy, the surface roughness of the workpiece to be plated are 0.06~0.1 μm.
9. the preparation method of any one graphene oxide/cobalt-based composite deposite according to claim 1~8, which is characterized in that
It comprises the following specific steps that:
S1. graphene oxide is prepared using Hummers method；
S2. cobalt salt, nickel salt, phosphate, boric acid, complexing agent and graphene oxide are dissolved in deionized water respectively, uses hydrogen-oxygen
The pH value for changing sodium and dilute sulfuric acid adjusting electroplate liquid is 2~6, and by ultrasonic vibration treatment, forms the composite plating of stable dispersion
Liquid；
S3. anode is cobalt, nickel or cobalt-nickel alloy, and cathode is workpiece to be plated, sets two interelectrode distances as 1~5cm, will be above-mentioned
Anode and cathode immerses in composite plating solution obtained by step S1, the ultrasonic vibration 10 in the ultrasonic vibrator that power is 50~100W
After~30min, electro-deposition is carried out using pulse current, graphene oxide/cobalt-based composite deposite is made on workpiece to be plated.
10. any one of the claim 1~8 graphene oxide/cobalt-based composite deposite is in automobile, machinery, precision manufactureing or boat
Application in its aviation field.
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| CN109652845A (en) * | 2019-01-18 | 2019-04-19 | 东华大学 | A kind of preparation method of graphene enhancing composite coating based on chromium |
| CN110424043A (en) * | 2019-07-10 | 2019-11-08 | 广东工业大学 | A kind of modified graphene oxide/cobalt-based composite deposite and its preparation method and application |
| CN111962111A (en) * | 2020-08-04 | 2020-11-20 | 深圳市生利科技有限公司 | Mobile phone material containing cobalt alloy coating and preparation method thereof |
| CN113174607A (en) * | 2021-04-29 | 2021-07-27 | 韩山师范学院 | Electrochemical preparation method of porous Ni-Co/graphene electrode |
| CN113355718A (en) * | 2021-06-08 | 2021-09-07 | 中国科学院兰州化学物理研究所 | MXene/GO composite coating and preparation method and application thereof |
| CN114942262A (en) * | 2022-02-25 | 2022-08-26 | 南京农业大学 | Laser-induced graphene electrode for detecting phosphate ions and preparation method |
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| CN110424043A (en) * | 2019-07-10 | 2019-11-08 | 广东工业大学 | A kind of modified graphene oxide/cobalt-based composite deposite and its preparation method and application |
| CN110424043B (en) * | 2019-07-10 | 2022-01-28 | 广东工业大学 | Modified graphene oxide/cobalt-based composite coating and preparation method and application thereof |
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| CN113174607B (en) * | 2021-04-29 | 2022-08-30 | 韩山师范学院 | Electrochemical preparation method of porous Ni-Co/graphene electrode |
| CN113355718A (en) * | 2021-06-08 | 2021-09-07 | 中国科学院兰州化学物理研究所 | MXene/GO composite coating and preparation method and application thereof |
| CN114942262A (en) * | 2022-02-25 | 2022-08-26 | 南京农业大学 | Laser-induced graphene electrode for detecting phosphate ions and preparation method |
| CN114942262B (en) * | 2022-02-25 | 2024-03-08 | 南京农业大学 | Laser-induced graphene electrode for phosphate ion detection and preparation method thereof |
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Application publication date: 20190101 |