CN103695877A - Method for preparing highly wear-resistant and corrosion-resistant carbon nano tube/graphene reinforced nickel-phosphorus based composite coating - Google Patents
Method for preparing highly wear-resistant and corrosion-resistant carbon nano tube/graphene reinforced nickel-phosphorus based composite coating Download PDFInfo
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Abstract
The invention relates to a method for preparing a highly wear-resistant and corrosion-resistant carbon nano tube/graphene reinforced nickel-phosphorus based composite coating. The method comprises specific steps of (1) weighting carbon nano tube and oxidized graphene according to the mass ratio of 1:1-10:1, adding into 500ml deionized water, stirring for 2 hours through ultrasonic so as to prepare carbon nano tube/oxidized graphene solution; (2) adding 50-200ml mixed solution into 500ml base liquid for chemical plating of nickel and phosphorus, adjusting pH value to be 4-5, immersing No.45 steel into the solution at 75-90 DEG C and plating for 1 hour; (3) washing and stoving the plated sample, then processing for 1 hour in nitrogen-hydrogen mixed gas at 400 DEG C, so as to obtain the carbon nano tube/graphene reinforced nickel-phosphorus based composite coating. In the method, the added oxidized graphene not only can eliminate the adverse impact on structure and properties caused by organic surfactant, but also can form a hybridization structure with the carbon nano tube so as to cooperatively reinforce the nickel-phosphorus coating, so that the nickel-phosphorus coating has more excellent wear resistance and corrosion resistance.
Description
Technical field
The present invention relates to a kind of carbon nanotube and as interpolation, strengthen mutually the preparation method of nickel phosphorus base chemical composite plating with Graphene.
Background technology
Along with high-tech development, need to there is high performance composite deposite, the performance of micron order composite deposite can not meet people's needs.Nano material has excellent performance, than common material, has higher hardness, wear resistance, self-lubricating patience and erosion resistance.Such as add the rigid particulates such as nano SiC, diamond, pottery in nickel-phosphor bath, can improve hardness and the surface compact of composite deposite, strengthen its wear resisting property and corrosion resistance nature; Toward the nanoparticle that adds MoS, graphite, PTFE etc. to there is self-lubricating property in nickel-phosphor bath, can make the composite deposite of self-lubricating property.Yet, although rigid particle add the wear resistance that can improve coating, also can bring damage to friction pair, and have self-lubricating property nanoparticle add the mechanical strength that membership reduces coating.
Since carbon nanotube is found, due to its novel structure and excellent performance, become rapidly the study hotspot in the fields such as domestic and international chemistry, physics and Materials science.Theoretical Calculation and experimental result show, the Young's modulus of carbon nanotube is 1.8 * 10
12pa, flexural strength is 14.2GPa, has superpower mechanical property; And calculate and also find that carbon nanotube is when stressed, can be by occurring that pentagon and heptagon, to discharging stress, show good self-lubricating property.
Utilize carbon nanotube to prepare nickel phosphorus base base composite cladding as wild phase, on the one hand even carbon nanotube is distributed in and in coating, is network commissure state, play dispersion-strengthened action, the cohesive force of compound phase and the hardness of composite deposite have been improved, cause antistick wearing and tearing ability to increase, strengthened flow resistance and the plow ability of coating, improved toughness and the ductility of composite deposite, coating difficult drop-off in wear process, has improved the wear resistance of composite deposite; Carbon nanotube is compound in nickel phosphorus matrix on the other hand, makes composite deposite surface microstructure projection, plays support loading effect, reduces the real contact area between composite deposite and friction pair, thereby cause friction resistance little in friction process, reduces frictional coefficient.
On the other hand, along with the wearing and tearing aggravation of composite deposite, part carbon nanotube will be rubbed to come off.These carbon nanotubes that come off play filling effect to concavo-convex friction surface in wear process, cover the protective membrane that forms one deck densification on surface of friction, have cut off directly contact between surface of friction.Carbon nanotube has tubular structure and high-strength and high-ductility and excellent self-lubricating property, plays " spot contact bearing " effect of support loading in friction process, has reduced frictional coefficient, has also improved the wear resisting property of composite deposite simultaneously.
Carbon nanotubes composite coatings also shows excellent corrosion resistance nature.The chemically reactive of carbon nanotube itself is very low, can acid-and base-resisting, the corrosion of salt, when its is wound around while covering grain surface, can be corrosive medium and crystal grain isolation, reduced the exposed area of anode in etchant solution, thus can the corrosion of mitigate corrosion solution to coating.Because even carbon nanotube is compounded in coating, stop the erosion rate of metallic nickel simultaneously, slowed down the increase of corrosion pit, reduced the size of corrosion pit.In addition; also because the current potential of carbon nanotube is corrected than the current potential of nickel; so when carbon nanotube is compound in nickel-base plating coat; nickel can be used as anode generation anodic polarization; further promote the passivating process of nickel; thereby reduced the corrosion of metallic nickel in corrosive medium, nickel coating is enhanced to the provide protection of matrix metal, thereby has improved the corrosion resistance nature of whole composite deposite.
Yet carbon nanotube is nano level material, under the effect of Van der Waals force, very easily reunite, be difficult to disperse.Therefore will bring into play the excellent properties of carbon nanotube, dispersed is the essential key issue solving in using.Traditional method is to add HS, makes it to be adsorbed on carbon nano tube surface, improves the stability of plating solution.But, the adding people and can reduce plating speed and the sticking power of coating to base material of tensio-active agent, and easily producing bubble in plating process, make surface generation pin hole or the hole of coating, thereby affect pattern and the quality of composite deposite.
Summary of the invention
The problem existing in order to overcome background technology, the object of the invention is to adopt graphene oxide as the dispersion agent of carbon nanotube, develops a kind of preparation method of carbon nanotube/Graphene composite deposite.Carbon nanotube and Graphene not only support and reach good dispersion effect mutually with a kind of hybrid structure form, and can also work in coordination with enhancing Ni-P coating, significantly improve wear resistance and the erosion resistance of coating.
The technical solution adopted in the present invention is:
1) ratio that is 1:1～10:1 in the mass ratio of carbon nanotube and graphene oxide weighs carbon nanotube and graphene oxide, amount to 2g, and add in 500ml deionized water, then stir ultrasonic dispersion 2h, make super homodisperse carbon nanotube/graphene oxide solution (A solution).
2) by following recipe configuration chemical nickel plating phosphor bath: six hydration nickel sulfate 30g/L, inferior sodium phosphate 32g/L, additive 80ml/L; After various materials are weighed, pour in two measuring cups, add deionized water to 500ml and be stirred well to solid matter and dissolve completely, obtain chemical plating fluid (B solution).
3) getting 50-200ml A solution joins in 500ml B solution, stirring, ultrasonic 1h, and to utilize sodium hydroxide to regulate pH value be 4-5, simultaneously keeping stirring, under ultrasonic condition, be warming up to 75-90 ℃. after temperature-stable, the 45# steel that is of a size of 40mm * 20 * 2.5mm is immersed in to plating 1h in solution.After taking out, wash, drying, insert in the tube-type atmosphere furnace that diameter is 6cm, 400 ℃, the middle 1h that processes of nitrogen hydrogen mixeding gas (flow is 100ml/min, and nitrogen hydrogen ratio is 5:1), obtain carbon nanotube/Graphene and strengthen nickel phosphorus base composite cladding.
The present invention adopts graphene oxide as the dispersion agent of carbon nanotube, without tensio-active agent in the situation that, realizes carbon nanotube/Graphene hybrid systems and is dispersed in plating solution, then realizes and plants and be embedded in nickel-phosphorus coating equably.Graphene oxide itself is with sp by monolayer carbon atom
2a kind of polynuclear plane of lining up that hydridization connects, a large amount of oxygen-containing functional groups is contained on surface, as hydroxyl, carboxyl, epoxy group(ing) etc.These functional groups can make graphene oxide have good wetting ability and dispersiveness.Meanwhile, in view of the constructional feature of carbon nanotube and graphene oxide, both will mutually be adsorbed and be formed a kind of hybrid structure by π key, not only stop the reunion of carbon nanotube, and it is curling to have stoped graphene oxide to occur.The more important thing is, graphene oxide is easily reduced into Graphene (rGO) in follow-up thermal treatment, and Graphene has the performances such as excellent mechanics, electricity, calorifics equally, itself is exactly comparatively ideal matrix material wild phase.Therefore the composite deposite that prepared by the present invention has higher hardness, and hardness can reach HV940, and higher than nickel-phosphorus coating 3-5 doubly, the antifriction quality that simultaneously also has nickel-phosphorus coating not possess, has considerable economic benefit and far-reaching social benefit for its wear resistance and erosion resistance.
Accompanying drawing explanation:
Fig. 1 is the electron scanning micrograph of the prepared carbon nanotube/Graphene chemical composite plating of embodiment 3;
Fig. 2 is the electron scanning micrograph of pure nickel phosphorus chemical plating;
Embodiment
Embodiment 1
The ratio that is 1:1 in the mass ratio of carbon nanotube and graphene oxide weighs carbon nanotube and graphene oxide, amount to 2g, and add in 500ml deionized water, then stir ultrasonic dispersion 2h, make super homodisperse carbon nanotube/graphene oxide solution (A solution).
Getting 100ml A solution joins in 500ml B solution, stirring, ultrasonic 1h, and to utilize sodium hydroxide to regulate pH value be 4-5, simultaneously keeping stirring, under ultrasonic condition, be warming up to 75-90 ℃. after temperature-stable, the 45# steel that is of a size of 40mm * 20 * 2.5mm is immersed in to plating 1h in solution.After taking out, wash, drying, insert in the tube-type atmosphere furnace that diameter is 6cm, 400 ℃, the middle 1h that processes of nitrogen hydrogen mixeding gas (flow is 100ml/min, and nitrogen hydrogen ratio is 5:1), obtain carbon nanotube/Graphene and strengthen nickel phosphorus base composite cladding.Coating hardness is HV765, and the bearing steel of take is right as friction, compares with pure nickel-phosphorus coating, and wear resistance improves 1.6 times, and erosion resistance improves 2.1 times.
Embodiment 2
The ratio that is 3:1 in the mass ratio of carbon nanotube and graphene oxide weighs carbon nanotube and graphene oxide, amount to 2g, and add in 500ml deionized water, then stir ultrasonic dispersion 2h, make super homodisperse carbon nanotube/graphene oxide solution (A solution).
Getting 100ml A solution joins in 500ml B solution, stirring, ultrasonic 1h, and to utilize sodium hydroxide to regulate pH value be 4-5, simultaneously keeping stirring, under ultrasonic condition, be warming up to 75-90 ℃. after temperature-stable, the 45# steel that is of a size of 40mm * 20 * 2.5mm is immersed in to plating 1h in solution.After taking out, wash, drying, insert in the tube-type atmosphere furnace that diameter is 6cm, 400 ℃, the middle 1h that processes of nitrogen hydrogen mixeding gas (flow is 100ml/min, and nitrogen hydrogen ratio is 5:1), obtain carbon nanotube/Graphene and strengthen nickel phosphorus base composite cladding.Coating hardness is HV840, and the bearing steel of take is right as friction, compares with pure nickel-phosphorus coating, and wear resistance improves 2.5 times, and erosion resistance improves 2.3 times.
Embodiment 3
The ratio that is 5:1 in the mass ratio of carbon nanotube and graphene oxide weighs carbon nanotube and graphene oxide, amount to 2g, and add in 500ml deionized water, then stir ultrasonic dispersion 2h, make super homodisperse carbon nanotube/graphene oxide solution (A solution).
Getting 100ml A solution joins in 500ml B solution, stirring, ultrasonic 1h, and to utilize sodium hydroxide to regulate pH value be 4-5, simultaneously keeping stirring, under ultrasonic condition, be warming up to 75-90 ℃. after temperature-stable, the 45# steel that is of a size of 40mm * 20 * 2.5mm is immersed in to plating 1h in solution.After taking out, wash, drying, insert in the tube-type atmosphere furnace that diameter is 6cm, 400 ℃, the middle 1h that processes of nitrogen hydrogen mixeding gas (flow is 100ml/min, and nitrogen hydrogen ratio is 5:1), obtain carbon nanotube/Graphene and strengthen nickel phosphorus base composite cladding.Coating hardness is HV940, and the bearing steel of take is right as friction, compares with pure nickel-phosphorus coating, and wear resistance improves 3.2 times, and erosion resistance improves 3.0 times.
Embodiment 4
The ratio that is 5:1 in the mass ratio of carbon nanotube and graphene oxide weighs carbon nanotube and graphene oxide, amount to 2g, and add in 500ml deionized water, then stir ultrasonic dispersion 2h, make super homodisperse carbon nanotube/graphene oxide solution (A solution).
Getting 150ml A solution joins in 500ml B solution, stirring, ultrasonic 1h, and to utilize sodium hydroxide to regulate pH value be 4-5, simultaneously keeping stirring, under ultrasonic condition, be warming up to 75-90 ℃. after temperature-stable, the 45# steel that is of a size of 40mm * 20 * 2.5mm is immersed in to plating 1h in solution.After taking out, wash, drying, insert in the tube-type atmosphere furnace that diameter is 6cm, 400 ℃, the middle 1h that processes of nitrogen hydrogen mixeding gas (flow is 100ml/min, and nitrogen hydrogen ratio is 5:1), obtain carbon nanotube/Graphene and strengthen nickel phosphorus base composite cladding.Coating hardness is HV820, and the bearing steel of take is right as friction, compares with pure nickel-phosphorus coating, and wear resistance improves 3.0 times, and erosion resistance improves 2.8 times.
Claims (3)
1. carbon nanotube/Graphene, as a preparation method for the nickel phosphorus base composite cladding of wild phase, is characterized in that, concrete steps are:
1) ratio that is 1:1～10:1 in the mass ratio of carbon nanotube and graphene oxide weighs carbon nanotube and graphene oxide, amount to 2g, and add in 500ml deionized water, then stir ultrasonic dispersion 2h, make super homodisperse carbon nanotube/graphene oxide solution (A solution).
2) by following recipe configuration chemical nickel plating phosphor bath: six hydration nickel sulfate 30g/L, inferior sodium phosphate 32g/L, additive 80ml/L; After various materials are weighed, pour in two measuring cups, add deionized water to 500ml and be stirred well to solid matter and dissolve completely, obtain chemical plating fluid (B solution).
3) getting 50-200ml A solution joins in 500ml B solution, stirring, ultrasonic 1h, and to utilize sodium hydroxide to regulate pH value be 4-5, simultaneously keeping stirring, under ultrasonic condition, be warming up to 75-90 ℃. after temperature-stable, the 45# steel that is of a size of 40mm * 20 * 2.5mm is immersed in to plating 1h in solution.After taking out, wash, drying, insert in the tube-type atmosphere furnace that diameter is 6cm, 400 ℃, the middle 1h that processes of nitrogen hydrogen mixeding gas (flow is 100ml/min, and nitrogen hydrogen ratio is 5:1), obtain carbon nanotube/Graphene and strengthen nickel phosphorus base composite cladding.
According to claim 1 carbon nanotube/Graphene as the preparation method of the nickel phosphorus base composite cladding of wild phase, it is characterized in that, described carbon nanotube is the multi-walled carbon nano-tubes after 90 ℃ of-100 ℃ of reflux 2h-4h process with nitration mixture, and wherein nitration mixture is that the analytical pure vitriol oil and concentrated nitric acid are the mixed acid of 3:1 according to volume ratio.
3. carbon nanotube/Graphene, as the preparation method of the nickel phosphorus base composite cladding of wild phase, is characterized in that according to claim 1, and described Graphene is that graphene oxide reduces and obtains after subsequent heat treatment.Graphene oxide is that natural scale graphite powder reacts 3h gained through the vitriol oil and potassium permanganate (mass ratio 10:1) at 90 ℃-100 ℃.
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| CN104726907A (en) * | 2015-03-25 | 2015-06-24 | 西南石油大学 | Nickel-tungsten graphene oxide (GO) composite plating solution, plated film and preparation method thereof |
| CN107099833A (en) * | 2017-03-29 | 2017-08-29 | 广东工业大学 | A kind of composite plating solution and preparation method thereof |
| CN107099834A (en) * | 2017-03-29 | 2017-08-29 | 广东工业大学 | A kind of copper radical self-lubricating composite coating and preparation method thereof |
| CN108277483A (en) * | 2018-02-01 | 2018-07-13 | 中国科学院宁波材料技术与工程研究所 | Graphene is co-deposited chemical nickel-plating liquid and its coating method |
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| CN110438496A (en) * | 2019-09-23 | 2019-11-12 | 兰州理工大学 | Vacuum cladding+chemical plating is molten-structure and preparation method thereof of plating composite coating |
| CN112441777A (en) * | 2019-08-30 | 2021-03-05 | 西安美刚达科技发展有限公司 | Nano fireproof material and preparation method thereof |
| CN112746197A (en) * | 2020-12-28 | 2021-05-04 | 江苏省特种设备安全监督检验研究院 | Preparation method of graphene-reinforced nickel-based nano composite powder metallurgy material |
| CN112831208A (en) * | 2020-12-30 | 2021-05-25 | 湖南金联星特种材料股份有限公司 | GO-CNTs synergistically enhanced hydrophobic polyurethane anticorrosive coating |
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Cited By (9)
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| CN110438496A (en) * | 2019-09-23 | 2019-11-12 | 兰州理工大学 | Vacuum cladding+chemical plating is molten-structure and preparation method thereof of plating composite coating |
| CN112746197A (en) * | 2020-12-28 | 2021-05-04 | 江苏省特种设备安全监督检验研究院 | Preparation method of graphene-reinforced nickel-based nano composite powder metallurgy material |
| CN112831208A (en) * | 2020-12-30 | 2021-05-25 | 湖南金联星特种材料股份有限公司 | GO-CNTs synergistically enhanced hydrophobic polyurethane anticorrosive coating |
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Application publication date: 20140402 |