CN109136915B - A kind of method of titanium-oxide-coated graphene oxide/aluminum matrix composite surface laser cladding - Google Patents
A kind of method of titanium-oxide-coated graphene oxide/aluminum matrix composite surface laser cladding Download PDFInfo
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- CN109136915B CN109136915B CN201811085903.9A CN201811085903A CN109136915B CN 109136915 B CN109136915 B CN 109136915B CN 201811085903 A CN201811085903 A CN 201811085903A CN 109136915 B CN109136915 B CN 109136915B
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- 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
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- 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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Abstract
A kind of method of titanium-oxide-coated graphene oxide/aluminum matrix composite surface laser cladding adsorbs Ti ion using hydro-thermal high pressure, and in the case where graphene oxide carries functional group's effect, and the GO@TiO of anatase titanium dioxide is obtained in after baking in water-less environment2Gained powder and Ti powder and glycerine adjust the mixed-powder for being mixed to get gluing state by a certain percentage, base aluminum 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, material is handled using laser melting coating later, obtains cladding material.Aluminium base surface cladding material friction coefficient is smaller handled by the present invention and has had both the features such as surface hardness is high, 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.
In fact, enhancing the intensity and other mechanical property of alumina-base material using carbon material such as carbon nanotube or graphene
The research of energy is carrying out always, and achieves a degree of progress.However, due to the physics such as its intensity extremely outstanding spy
Property, people ignore its excellent attribute in material abrasiveness and hardness instead.A large number of studies show that the correct choosing of reinforced phase
Select the wear-resisting property and hardness that can directly improve composite material.And graphene oxide (GO) is due to the essential attribute of its carbon material,
Natural succession its self-lubricating and preferable thermal diffusivity etc. are different from the speciality of other reinforcing materials.Thus correctly use can
Efficiently reduce the loss of 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 reinforced aluminum matrix composites preparation and forming skill at present
Art.
Summary of the invention
In order to overcome conventional oxidation graphene composite material to prepare molding technological difficulties, the object of the present invention is to provide one
Kind enhances the melting and coating technique of aluminium base surface abrasion resistance using graphene oxide.It is to add mixed-powder in substrate surface, is utilized
The laser of certain power forms powder itself or forms a protective layer with matrix chemical combination.It is compared to traditional table such as plating
Surface treatment technique, it has many advantages, such as, such as applicable basis material range of choice is wide, cladding layer controllability is high, customization performance
By force, excellent bonding performance etc..
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:
3TiO2 + 7Al→3TiAl +2Al2O3(1)
Ti3Al+2Al → 3TiAl (2)
By introducing titanium oxide or titanium elements on aluminum substrate surface, titanium directly react with aluminium between generation titanium aluminium at high temperature
Compound.And using the self-lubricating and extremely strong thermal conductivity of graphene oxide, so that the surface hardness straight line of material improves, together
When effectively reduce the coefficient of friction of material surface.
The present invention is achieved by the following technical solutions.
A kind of method of titanium-oxide-coated graphene oxide/aluminum matrix composite surface laser cladding of the present invention,
Include 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 anhydrous
Vapour.The proportion of graphene oxide and ethyl alcohol is 0.2 ~ 0.4g: 50ml.
(2) glycerine and tetraisopropyl titanate composition will be poured into through step (1) pretreated graphene oxide dispersion
Precursor liquid in seal, and again be ultrasonically treated 1 ~ 1.5h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.4
~1.2。
(3) forerunner's suspension through step (2) is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product of reaction kettle
35%~70%.Reaction kettle is integrally put into reacting furnace again and is heated, is warming up to 70~110 DEG C with 1~5 DEG C/min, heat preservation 1~
2h, then after being warming up to 175 ~ 180 DEG C with 1~3 DEG C/min, take out reaction kettle after keeping the temperature 10~15h；Reaction kettle should be air-cooled to room
Warm rear is openable.
(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 needle-shaped anatase type titanium oxide coating can be obtained.
(6) powder obtained by step (5) is put into beaker and a certain amount of titanium valve is added, and be added a certain amount of the third three
Alcohol, the mass ratio of titanium valve and graphene oxide is 14.5 ~ 17:1 among these.It is 2 ~ 4.5% that glycerine, which accounts for total volume ratio, is stomata
The key of control, then with ultrasonic treatment one hour, which should keep preferable aridity, finally obtain gluing state
Mixed-powder.
(7) base aluminum 1500 ~ 2000# sand paper is polished, alcohol washes drying mixes gluing state obtained by step (6)
Powder is uniformly applied to matrix surface, and prefabricated thickness control is 0.7 ~ 1.2mm.Again with flame gun Quick uniform presintering powder 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 0.7 ~ 0.9Kw, and scanning speed is 5.5 ~ 8mm/s, and spot diameter is 3 ~ 5mm, among these,
Inclination 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) there is the graphene oxide of transition zone on alumina-base material surface and matrix knot
It closes, while there is more preferable interface, further reduces graphene oxide reunion probability.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1.
By graphene oxide in the analysis straight alcohol clock 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 by gained dispersion liquid pour into glycerine and tetraisopropyl titanate composition precursor liquid in seal
It is ultrasonically treated 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.4.Hydro-thermal process is carried out later, wherein hanging
Turbid volume accounts for the molten product 50% of reaction kettle.It places into reacting furnace and heats, be warming up to 90 DEG C with 5 DEG C/min, keep the temperature 2h, then with 3
DEG C/after min is warming up to 180 DEG C, keep the temperature 10h.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.Afterwards by 450 DEG C under protection of argon gas of gained powder
Middle roasting.Time controls in 2h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.
Gained powder and titanium valve are matched in beaker later, and a certain amount of glycerine is added, among these titanium valve and oxygen
The mass ratio of graphite alkene is 16:1.It is 2% that glycerine, which accounts for total volume ratio, and processing whole process then uses ultrasonic treatment one without steam
Hour.Obtain the mixed-powder of gluing state.Base aluminum A356 1500 ~ 2000# sand paper is polished, alcohol washes drying.Institute
It obtains gluing state mixed-powder and is uniformly applied to matrix surface, prefabricated thickness control is 0.7mm.The pre-burning of flame gun Quick uniform is used again
Powder is tied in matrix surface.Material is handled using laser melting coating in argon gas guard box later.Its process parameter control
Are as follows: laser power 0.7Kw, scanning speed 6mm/s, spot diameter 3mm, among these, inclination angle control are 20 °.As a result
Show to be compared to simple plating titanium valve, coefficient of friction, which carries, drops to 0.38 or so by 0.43 under specific load.
Embodiment 2.
By graphene oxide in the analysis straight alcohol clock pre-dispersed 3h of ultrasound, temperature is room temperature, and whole-process control is without steam.Proportion
Be strict controlled in 0.2g:50ml, after by gained dispersion liquid pour into glycerine and tetraisopropyl titanate composition precursor liquid in seal
It is ultrasonically treated 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.8.Hydro-thermal process is carried out later, wherein hanging
Turbid volume accounts for the molten product 50% of reaction kettle.It places into reacting furnace and heats, be warming up to 90 DEG C with 3 DEG C/min, keep the temperature 1h, then with 2
DEG C/after min is warming up to 180 DEG C, keep the temperature 12h.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.Afterwards by 450 DEG C under protection of argon gas of gained powder
Middle roasting.Time controls in 1h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.
Gained powder and titanium valve are matched in beaker later, and a certain amount of glycerine is added, among these titanium valve and oxygen
The mass ratio of graphite alkene is 16:1.It is 3% that glycerine, which accounts for total volume ratio, and processing whole process then uses ultrasonic treatment one without steam
Hour.Obtain the mixed-powder of gluing state.Base aluminum ZL105 1500 ~ 2000# sand paper is polished, alcohol washes drying.Institute
It obtains gluing state mixed-powder and is uniformly applied to matrix surface, prefabricated thickness control is 0.7mm.The pre-burning of flame gun Quick uniform is used again
Powder is tied in matrix surface.Material is handled using laser melting coating in argon gas guard box later.Its process parameter control
Are as follows: laser power 0.8Kw, scanning speed 7mm/s, spot diameter 4mm, among these, inclination angle control are 25 °.As a result
Show to be compared to simple plating titanium valve, coefficient of friction drops to 0.37 or so by 0.43 under specific load.
Embodiment 3.
By graphene oxide in the analysis straight alcohol clock pre-dispersed 2h of ultrasound, temperature is room temperature, and whole-process control is without steam.Proportion
Be strict controlled in 0.4g:50ml, after by gained dispersion liquid pour into glycerine and tetraisopropyl titanate composition precursor liquid in seal
It is ultrasonically treated 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.4.Hydro-thermal process is carried out later, wherein hanging
Turbid volume accounts for the molten product 60% of reaction kettle.It places into reacting furnace and heats, be warming up to 100 DEG C with 1 DEG C/min, keep the temperature 2h, then with 3
DEG C/after min is warming up to 180 DEG C, keep the temperature 10h.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.Afterwards by 500 DEG C under protection of argon gas of gained powder
Middle roasting.Time controls in 1h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.
Gained powder and titanium valve are matched in beaker later, and a certain amount of glycerine is added, among these titanium valve and oxygen
The mass ratio of graphite alkene is 16:1.It is 2% that glycerine, which accounts for total volume ratio, and processing whole process then uses ultrasonic treatment one without steam
Hour.Obtain the mixed-powder of gluing state.Base aluminum 1500 ~ 2000# sand paper is polished, alcohol washes drying.Gained glue
Glutinous state mixed-powder is uniformly applied to matrix surface, and prefabricated thickness control is 0.7mm.Powder is pre-sintered with flame gun Quick uniform again
End is in matrix surface.Material is handled using laser melting coating in argon gas guard box later.Its process parameter control are as follows: swash
Optical power is 0.9Kw, scanning speed 7mm/s, spot diameter 5mm, and among these, inclination angle control is 30 °.The result shows that phase
It is compared to plate titanium valve merely, under specific load, coefficient of friction is by 0.43 decline equally to 0.357 or so.
Claims (1)
1. a kind of method of titanium-oxide-coated graphene oxide/aluminum matrix composite surface laser cladding, it is characterized in that include with
Lower step:
(1) by graphene oxide in analysis straight alcohol the pre-dispersed 1 ~ 3h of ultrasound, temperature is room temperature, and whole-process control is without steam, oxygen
The proportion of graphite alkene and ethyl alcohol is 0.2 ~ 0.4g: 50mL；
(2) before glycerine and tetraisopropyl titanate composition will be poured into through step (1) pretreated graphene oxide dispersion
It drives in liquid and seals, and be ultrasonically treated 1 ~ 1.5h again, glycerine and tetraisopropyl titanate volume ratio are 10:0.4 ~ 1.2；
(3) forerunner's suspension through step (2) is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product 35% of reaction kettle
~70%；Reaction kettle is integrally put into reacting furnace again and is heated, is warming up to 70~110 DEG C with 1~5 DEG C/min, keeps the temperature 1~2h, then
After being warming up to 175 ~ 180 DEG C with 1~3 DEG C/min, reaction kettle is taken out after keeping the temperature 10~15h；Reaction kettle is air-cooled to room temperature；
(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,
The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained in 1 ~ 3h in time control；
(6) powder obtained by step (5) is put into beaker and is added titanium valve and glycerine, the mass ratio of titanium valve and graphene oxide
For 14.5 ~ 17:1, it is 2 ~ 4.5% that glycerine, which accounts for total volume ratio, is subsequently ultrasonicated for one hour, mixes powder process and keeps drying, finally
Obtain the mixed-powder of gluing state；
(7) base aluminum 1500 ~ 2000# sand paper is polished, alcohol washes drying, gluing state mixed-powder obtained by step (6)
It is uniformly applied to matrix surface, prefabricated thickness control is 0.7 ~ 1.2mm, then with flame gun Quick uniform presintering powder 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 0.7 ~ 0.9kW, and scanning speed is 5.5 ~ 8mm/s, and spot diameter is 3 ~ 5mm, inclination angle control
It is 20 ~ 35 °；
Hydrothermal reaction kettle liner described in step (3) is polytetrafluoroethylene (PTFE).
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| CN113088957B (en) * | 2021-02-20 | 2022-09-02 | 景德镇明兴航空锻压有限公司 | Method for preparing wear-resistant and high-temperature-resistant coating on surface of titanium alloy through laser cladding |
| CN115491659A (en) * | 2022-11-01 | 2022-12-20 | 西北工业大学 | Method for improving mechanical property of metal-based composite material by modifying graphene on surface of titanium dioxide |
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| CN102496700A (en) * | 2011-12-20 | 2012-06-13 | 中国科学院新疆理化技术研究所 | Graphene-titanium dioxide nanotube composite material and preparation method thereof |
| CN106532014A (en) * | 2016-12-26 | 2017-03-22 | 天津大学 | Method for preparing composite material that stannic oxide nano-particles attach to graphene oxide |
| KR20180057323A (en) * | 2016-11-22 | 2018-05-30 | 재단법인 한국탄소융합기술원 | Method of manufacturing metal-loaded TiO2/graphene composites through one-pot hydrothermal synthesis and the TiO2/graphene composites manufactured by the same |
| CN108127123A (en) * | 2018-01-16 | 2018-06-08 | 武汉理工大学 | A kind of composite coating material applied to semimetal iron-based brake block and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102496700A (en) * | 2011-12-20 | 2012-06-13 | 中国科学院新疆理化技术研究所 | Graphene-titanium dioxide nanotube composite material and preparation method thereof |
| KR20180057323A (en) * | 2016-11-22 | 2018-05-30 | 재단법인 한국탄소융합기술원 | Method of manufacturing metal-loaded TiO2/graphene composites through one-pot hydrothermal synthesis and the TiO2/graphene composites manufactured by the same |
| CN106532014A (en) * | 2016-12-26 | 2017-03-22 | 天津大学 | Method for preparing composite material that stannic oxide nano-particles attach to graphene oxide |
| CN108127123A (en) * | 2018-01-16 | 2018-06-08 | 武汉理工大学 | A kind of composite coating material applied to semimetal iron-based brake block and preparation method thereof |
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