CN109183024A - A kind of laser cladding on alumina-coated graphene oxide/mg-based material surface - Google Patents
A kind of laser cladding on alumina-coated graphene oxide/mg-based material surface Download PDFInfo
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- CN109183024A CN109183024A CN201811083470.3A CN201811083470A CN109183024A CN 109183024 A CN109183024 A CN 109183024A CN 201811083470 A CN201811083470 A CN 201811083470A CN 109183024 A CN109183024 A CN 109183024A
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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Abstract
A kind of laser cladding on alumina-coated graphene oxide/mg-based material surface adsorbs Al ion using hydro-thermal high pressure, and in the case where graphene oxide carries functional group's effect, and γ type GO@aluminium oxide is obtained in after baking in water-less environment.Gained powder and Fe powder, Si powder and glycerine certain proportion adjust the mixed-powder for being mixed to get gluing state.Matrix alloy magnesium is polished with sand paper, and gluing state mixed-powder is uniformly applied to matrix face.Again with flame gun Quick uniform presintering powder in matrix surface.Then material is handled using laser melting coating.Aluminium base surface cladding material wear rate handled by the present invention is low and has had both the features such as high reinforced phase associativity of surface hardness is good, meanwhile, the present invention has many advantages, such as that simple, safety, low cost are easily operated and controllable.
Description
Technical field
The invention belongs to technical field of material.
Background technique
The two-dimensional material for the monoatomic layer thickness that graphene nanometer sheet is made of sp2 hydbridized carbon atoms, shows one
The unusual physical property of series.Graphene nanometer sheet causes physics, chemistry and materialogy because of its special two-dimensional structure
The great interest of boundary researcher, basic research and engineering Application Research in relation to graphene become research hotspot in recent years.
Since graphene has high intensity, tensile strength up to 130GPa, imply graphene have in material application study it is huge
Big application space.
Enhance using carbon material such as carbon nanotube or graphene the intensity and other mechanical properties of metal_based material
Research achieves a degree of progress.However, due to physical characteristics such as its intensity extremely outstanding, people ignore it in material
Excellent attribute in grinding abrasion and hardness.A large number of studies show that the correct selection of reinforced phase can directly improve composite material
Wear-resisting property and hardness.And graphene oxide (GO) is due to the essential attribute of its carbon material, its self-lubricating of natural succession and
Preferable thermal diffusivity etc. is different from the speciality of other reinforcing materials.Thus correctly using the loss that can efficiently reduce material.
The defect of right graphene oxide is also more obvious.Graphene oxide shows very poor profit similar to the structure of CNT
Moist, this directly results in not strong with aluminum substrate interfacial bonding property, is unfavorable for the preparation of composite material.Thus, improve itself and base
The wetability of body simultaneously selects correct process to become the key using graphene enhancing alumina-base material abrasion.
Graphene oxide, which improves wetability method, at present overlay coating etc., and such as chemical nickel plating, this method is mainly by carboxylic
The graphene of base is through sensitization plays, after activation, is put into plating in chemical plating fluid, as the progress of reaction can be in graphene oxide table
Face obtains graininess coating, but expensive, and commonly uses toxic reagent, not environmentally and high production cost, is not suitable for extensive
Production.
In publication CN106148949A, title are as follows: a kind of " laser-induction composite cladding graphene enhancing Ni3Ti
In the method for composite material ".Graphene is pre-processed using chemical plating to obtain the graphene of nickel plating.Powder is mixed again carries out routine
It is laser sintered.In fact this method due to chemical plating limitation, it is larger to human injury, and it also requires individually to graphene
Carboxylated, the production cycle is long, while utilizing is sintering process of dusting, higher for such powder waste degree, has certain office
It is sex-limited.
Therefore, still lack a kind of cost-effective graphene oxide enhancing magnesium-based composite material surface abrasion performance at present
Surface coating technique.
Summary of the invention
In order to overcome conventional oxidation graphene composite material to prepare molding technological difficulties, the present invention, which provides, a kind of utilizes oxygen
The melting and coating technique of graphite alkene enhancing aluminium base surface abrasion resistance.It is to add mixed-powder in substrate surface, utilizes certain power
Laser make powder itself formed or with matrix chemical combination formed a protective layer.It is compared to the conventional surfaces such as plating processing work
Skill, it has many advantages, such as, such as applicable basis material range of choice is wide, cladding layer controllability is high, customization performance is strong, associativity
It can wait well.
Laser cladding technology includes selection proportion, the control of environment and the determination of the technological parameter three crucial rings of powder
Section, these three links are all linked with one another, all directly affect the quality of product.
In the present invention, graphene oxide is pre-processed using hydro-thermal method, the rear gluing state for recycling glycerine is protected
The adhesion for holding its dispersibility and material reaches during the mixed powder of reduction due to inhomogeneities caused by different densities.
Concrete principle of the invention are as follows:
3Mg + 4Al2O3 = 3MgAl2O4 + 2Al
By introducing aluminium oxide on magnesium matrix surface, aluminium oxide is directly reacted with magnesium at high temperature generates spinelle.And utilize oxygen
The self-lubricating of graphite alkene and extremely strong thermal conductivity simultaneously effective reduce so that the surface hardness straight line of material improves
Material surface abrasion.
The present invention is achieved by the following technical solutions.
A kind of method of alumina-coated graphene oxide cladding magnesium alloy substrate of the present invention, including following step
Suddenly.
(1) by graphene oxide in analysis straight alcohol the pre-dispersed 1 ~ 3h of ultrasound, temperature is room temperature, and whole-process control is anhydrous
Vapour.Proportion is strict controlled in 0.2 ~ 0.4g: 50ml.
(2) before acetylacetone,2,4-pentanedione and aluminum nitrate composition will be poured into through step (1) pretreated graphene oxide dispersion
It drives in liquid and seals, and be ultrasonically treated 1 ~ 2h again.Among these, acetylacetone,2,4-pentanedione and aluminum nitrate (Al (NO3)3) proportion be 0.2 ~ 0.4:
1mol。
(3) forerunner's suspension through step (2) is imported in hydrothermal reaction kettle, wherein graphene oxide: aluminum nitrate proportion
For 1:1 ~ 1.2mol, suspension volume accounts for the molten product 35%~70% of reaction kettle.It places into reacting furnace and heats, with 1~5 DEG C/min liter
Temperature keeps the temperature 1~2h to 50~80 DEG C, then after being warming up to 150 ~ 160 DEG C with 1~3 DEG C/min, keeps the temperature 3~5h；It takes out, reaction kettle
It seals air-cooled.
(4) being taken out through solution obtained by step (3), centrifugal treating, and be repeatedly centrifuged by pouring into analysis straight alcohol to molten
Body is colourless, and revolving speed is controlled in 9000 ~ 16000rpm.Whole process sealing guarantees without steam.
(5) the mixed-powder vacuum drying that step (4) is obtained, after will be in the powder under protection of argon gas 450 ~ 500 DEG C
Roasting.Time controls in 1 ~ 3h.The graphene oxide that surface has gama-alumina coating can be obtained.
(6) powder obtained by step (5) is put into beaker and a certain amount of fine silica powder and iron powder is added, and be added a certain amount of
Glycerine, wherein silicon powder control is total powder quality 4 ~ 8%, and the mass ratio of graphene oxide is 4 ~ 7%, and surplus is atomized aluminium,
Size Control is 5 ~ 30 μm.It is 2 ~ 6% to reduce stomata that glycerine, which accounts for total volume ratio, and processing whole process then uses ultrasound without steam
Processing 1 hour, obtains the mixed-powder of gluing state.
(7) matrix mg-based material alloy sheets 1500 ~ 2000# sand paper is polished, alcohol washes drying.After will be step
(6) gained gluing state mixed-powder is uniformly applied to matrix surface, and prefabricated thickness control is 0.7 ~ 1.2mm.It is fast with flame gun again
Fast uniformly presintering powder is in matrix surface.
(8) step (7) resulting materials are put into argon gas guard box, material is handled using laser melting coating.Its work
Skill state modulator are as follows: laser power is 0.5 ~ 1.2Kw, and scanning speed is 5 ~ 8mm/s, and spot diameter is that 2 ~ 5mm inclines among these
Oblique angle is more crucial, and controlling is 20 ~ 35 °.
Hydrothermal reaction kettle liner described in step (3) of the present invention is polytetrafluoroethylene (PTFE).
The present invention have following technical effect that (1) the method reduce in conventional blending processes of powders since density variation causes
Lamination.(2) the conventional caused dust pollution that dusts can be reduced using the viscosity of lipid itself, it is more environmentally-friendly.(3)
This method reaction temperature is lower, and danger coefficient is low.(4) graphene oxide of transition zone reacts on alumina-base material surface with matrix
Spinel structure is formed, while there is more preferable interface, further reduces graphene oxide reunion probability.(5) graphite oxide
Alkene coating has a degree of protective effect to the high temperature of laser.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1:
By graphene oxide in analysis straight alcohol the pre-dispersed 1h of ultrasound, temperature is room temperature, and whole-process control is without steam.Proportion is stringent
Control in 0.2g:50ml, after the precursor liquid of acetylacetone,2,4-pentanedione and aluminum nitrate composition imported into sealing ultrasonic treatment 1h in dispersion liquid.This
Wherein, acetylacetone,2,4-pentanedione and aluminum nitrate (Al (NO3)3) match as 0.2:1mol.Hydro-thermal process is carried out later, wherein suspension volume
Account for the molten product 50% of reaction kettle.It places into reacting furnace and heats, be warming up to 80 DEG C with 5 DEG C/min, keep the temperature 2h, then with 3 DEG C/min heating
To after 160 DEG C, 5h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into analysis straight alcohol
Repeatedly centrifugation is colourless to solution.Whole process sealing guarantees without steam.It will be roasted in gained powder under protection of argon gas 450 DEG C afterwards.When
Between control in 2h.Surface, which can be obtained, has γ-Al with surface can be obtained2O3The graphene oxide of coating.
Gained powder and iron powder, silicon powder are matched in beaker later, and a certain amount of glycerine is added, among these silicon powder
Control is total powder quality 4%, and the mass ratio of GO is 5%, and surplus is atomized aluminium, and size Control is 5 μm.Glycerine accounts for total volume ratio
It is 2 ~ 6%, processing whole process is then used ultrasonic treatment one hour without steam.Obtain the mixed-powder of gluing state.By base aluminum
AM60 is polished with 1500 ~ 2000# sand paper, alcohol washes drying.Gained gluing state mixed-powder is uniformly applied to matrix surface,
Prefabricated thickness control is 0.7mm.Again with flame gun Quick uniform presintering powder in matrix surface.Later in argon gas guard box
Material is handled using laser melting coating.Its process parameter control are as follows: laser power 0.7Kw, scanning speed 6mm/s,
Spot diameter is 3mm, and among these, inclination angle control is 20 °.
Embodiment 2.
By graphene oxide in analysis straight alcohol the pre-dispersed 1h of ultrasound, temperature is room temperature, and whole-process control is without steam.Proportion
Be strict controlled in 0.2g:50ml, after will acetylacetone,2,4-pentanedione and aluminum nitrate composition precursor liquid import dispersion liquid in seal ultrasonic treatment
1h.Among these, acetylacetone,2,4-pentanedione and aluminum nitrate (Al (NO3)3) match as 0.3:1mol.Hydro-thermal process is carried out later, wherein suspension
Volume accounts for the molten product 60% of reaction kettle.It places into reacting furnace and heats, be warming up to 60 DEG C with 3 DEG C/min, keep the temperature 2h, then with 3 DEG C/min
After being warming up to 150 DEG C, 3h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and pure by pouring into analysis
Ethyl alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.It will be roasted in gained powder under protection of argon gas 500 DEG C afterwards
It burns.Time controls in 1h.Surface, which can be obtained, has γ-Al with surface can be obtained2O3The graphene oxide of coating.
Gained powder and iron powder, silicon powder are matched in beaker later, and a certain amount of glycerine is added, among these silicon powder
Control is total powder quality 6%, and the mass ratio of graphene oxide is 6%, and surplus is atomized aluminium, and size Control is about 15 μm.The third three
It is 3% that alcohol, which accounts for total volume ratio, and processing whole process is then used ultrasonic treatment one hour without steam.Obtain the mixed-powder of gluing state.
Base aluminum AZ61 1500 ~ 2000# sand paper is polished, alcohol washes drying.Gained gluing state mixed-powder is uniformly applied to
Matrix surface, prefabricated thickness control are 0.9mm.Again with flame gun Quick uniform presintering powder in matrix surface.Later in argon
Material is handled using laser melting coating in gas shielded case.Its process parameter control are as follows: laser power 0.9Kw, scanning speed
Degree is 7mm/s, spot diameter 4mm, and among these, inclination angle control is 25 °.
Embodiment 3.
By graphene oxide in analysis straight alcohol the pre-dispersed 1h of ultrasound, temperature is room temperature, and whole-process control is without steam.Proportion
Be strict controlled in 0.2g:50ml, after will acetylacetone,2,4-pentanedione and aluminum nitrate composition precursor liquid import dispersion liquid in seal ultrasonic treatment
1h.Among these, acetylacetone,2,4-pentanedione and aluminum nitrate (Al (NO3)3) match as 0.4:1mol.Hydro-thermal process is carried out later, wherein suspension
Volume accounts for the molten product 40% of reaction kettle.It places into reacting furnace and heats, be warming up to 80 DEG C with 3 DEG C/min, keep the temperature 1h, then with 2 DEG C/min
After being warming up to 160 DEG C, 3h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and pure by pouring into analysis
Ethyl alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.It will be roasted in gained powder under protection of argon gas 480 DEG C afterwards
It burns.Time controls in 2h.Surface, which can be obtained, has γ-Al with surface can be obtained2O3The graphene oxide of coating.
Gained powder and iron powder, silicon powder are matched in beaker later, and a certain amount of glycerine is added, among these silicon powder
Control is total powder quality 7%, and the mass ratio of GO is 5%, and surplus is atomized aluminium, and size Control is about 10 μm.Glycerine accounts for totality
For product than being 6%, processing is whole without steam, and then with ultrasonic treatment one hour.Obtain the mixed-powder of gluing state.By matrix
AZ91D is polished with 1500 ~ 2000# sand paper, alcohol washes drying.Gained gluing state mixed-powder is uniformly applied to matrix table
Face, prefabricated thickness control are 1.1mm.Again with flame gun Quick uniform presintering powder in matrix surface.It is protected later in argon gas
Material is handled using laser melting coating in case.Its process parameter control are as follows: laser power 1.2Kw, scanning speed are
8mm/s, spot diameter 5mm, among these, inclination angle control are 30 °.
Claims (1)
1. a kind of laser cladding on alumina-coated graphene oxide/mg-based material surface, comprising the following steps:
(1) by graphene oxide in analysis straight alcohol the pre-dispersed 1 ~ 3h of ultrasound, temperature is room temperature, and whole-process control is matched without steam
Than being strict controlled in 0.2 ~ 0.4g: 50ml；
(2) precursor liquid of acetylacetone,2,4-pentanedione and aluminum nitrate composition will be poured into through step (1) pretreated graphene oxide dispersion
Middle sealing, and it is ultrasonically treated 1 ~ 2h again, acetylacetone,2,4-pentanedione and aluminum nitrate proportion are 0.2 ~ 0.4:1mol；
(3) forerunner's suspension through step (2) is imported in hydrothermal reaction kettle, wherein graphene oxide: aluminum nitrate proportion is
1:1 ~ 1.2mol, suspension volume account for the molten product 35%~70% of reaction kettle；It places into reacting furnace and heats, with 1~5 DEG C/min heating
To 50~80 DEG C, 1~2h is kept the temperature, then after being warming up to 150 ~ 160 DEG C with 1~3 DEG C/min, keeps the temperature 3~5h；It takes out, reaction kettle is close
It seals air-cooled；
(4) being taken out through solution obtained by step (3), centrifugal treating, and by pour into analysis straight alcohol be repeatedly centrifuged to solution without
Color, revolving speed control guarantee in 9000 ~ 16000rpm, whole process sealing without steam；
(5) the mixed-powder vacuum drying that step (4) is obtained, after will be roasted in the powder under protection of argon gas 450 ~ 500 DEG C,
Time controls in 1 ~ 3h；The graphene oxide that surface has gama-alumina coating can be obtained；
(6) powder obtained by step (5) is put into beaker and fine silica powder and iron powder is added, and glycerine is added, wherein silicon powder controls
For total powder quality 4 ~ 8%, the mass ratio of graphene oxide is 4 ~ 7%, and surplus is atomized aluminium, and size Control is 5 ~ 30 μm；The third three
It is 2 ~ 6% to reduce stomata that alcohol, which accounts for total volume ratio, and processing whole process obtained gluing state with ultrasonic treatment 1 hour without steam, and then
Mixed-powder；
(7) matrix mg-based material alloy sheets 1500 ~ 2000# sand paper is polished, alcohol washes drying then will be step (6)
Gained gluing state mixed-powder is uniformly applied to matrix surface, and prefabricated thickness control is 0.7 ~ 1.2mm, then quickly equal with flame gun
Even presintering powder is in matrix surface；
(8) step (7) resulting materials are put into argon gas guard box, material is handled using laser melting coating, technique ginseng
Numerical control is made as: laser power is 0.5 ~ 1.2Kw, and scanning speed is 5 ~ 8mm/s, and spot diameter is 2 ~ 5mm, among these, inclination angle
More crucial, controlling is 20 ~ 35 °；
Hydrothermal reaction kettle liner described in step (3) is polytetrafluoroethylene (PTFE).
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| CN109942296A (en) * | 2019-01-11 | 2019-06-28 | 南京工业大学 | High-thermal-conductivity insulating graphene/aluminum oxide/aluminum composite material and preparation method thereof |
| CN110295298A (en) * | 2019-01-17 | 2019-10-01 | 杭州电缆股份有限公司 | A kind of preparation method of graphene aluminium composite material |
| CN113426997A (en) * | 2021-06-11 | 2021-09-24 | 西安交通大学 | High-specific-gravity tungsten-nickel-iron alloy and laser additive manufacturing method thereof |
| CN114921699A (en) * | 2022-05-26 | 2022-08-19 | 扬州工业职业技术学院 | High-temperature-resistant composite material for wheel hub and wheel hub |
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| CN113426997A (en) * | 2021-06-11 | 2021-09-24 | 西安交通大学 | High-specific-gravity tungsten-nickel-iron alloy and laser additive manufacturing method thereof |
| CN114921699A (en) * | 2022-05-26 | 2022-08-19 | 扬州工业职业技术学院 | High-temperature-resistant composite material for wheel hub and wheel hub |
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