CN109161887B - A kind of coated with titanium oxide/graphene oxide surface of steel plate coating cladding ultrasonic method - Google Patents
A kind of coated with titanium oxide/graphene oxide surface of steel plate coating cladding ultrasonic method Download PDFInfo
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- CN109161887B CN109161887B CN201811083850.7A CN201811083850A CN109161887B CN 109161887 B CN109161887 B CN 109161887B CN 201811083850 A CN201811083850 A CN 201811083850A CN 109161887 B CN109161887 B CN 109161887B
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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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Abstract
A kind of coated with titanium oxide/graphene oxide surface of steel plate coating cladding ultrasonic method adsorbs Ti ion using hydro-thermal high pressure, and in the case where graphene oxide carries functional group's effect, and anatase titanium dioxide GO@TiO2(anatase titanium dioxide is obtained in after baking in water-less environment).The thin iron powder of gained powder and Ti powder, Si powder and surplus adjusts the mixed-powder for being mixed to get gluing state with glycerine certain proportion.Steel plate 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 handle using laser melting coating in atmosphere and further disperse reinforced phase under the synergistic effect of high-energy ultrasonic.Surface of steel plate cladding material wear rate handled by the present invention is low, surface hardness is high, while 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.
Intensity and other mechanical properties for enhancing metal material using carbon material such as carbon nanotube or graphene are current
Belong to forward position research contents.Document shows that the correct selection of reinforced phase can directly improve the wear-resisting property and hardness of 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 no
It is same as the speciality of other reinforcing materials, correctly use can efficiently reduce the abrasion of material surface and increase the hardness of material.
Material will be made to have preferable wearability using graphene as the overlay coating of metal material, self-lubrication then can be compound
The stability of material abrasion is directly promoted in the wear process of material.
The defect of right graphene oxide or graphene is also more obvious.Graphene oxide is showed similar to the structure of CNT
Very poor wetability out, this directly results in not strong and hold in preparation or galvanization process with metallic matrix interfacial bonding property
It is easy to reunite.This is all unfavorable for the progress of composite material surface coating.Thus, improve the wetability of itself and matrix and selects correct
Process becomes the key using graphene reinforced metal-matrix composite wear-resisting property.
On the other hand, high-energy ultrasonic dispersion may make melt to generate acoustic pressure as a kind of novel Dispersion of Reinforcement technology
Gradient simultaneously leads to instantaneous high pressure and microjet in melt, is effectively facilitated the dispersion of reinforced phase.Simultaneously as caused by ultrasound
Local temperature increases and molecular motion accelerated energy reduces the viscosity and surface tension of reinforced phase, it is thus possible to mention to a certain extent
The wetability of high melt and reinforced phase.
Graphene, which improves wetability method, at present overlay coating etc., and such as chemical nickel plating, this method is mainly by carboxylated
Graphene through sensitization plays, after activation, plating in chemical plating fluid is put into, as the progress of reaction can be in carboxylated graphene surface
Graininess coating is obtained, but expensive, and commonly use toxic reagent, not environmentally and high production cost, is not suitable for extensive raw
It produces.
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, in conclusion still lacking a kind of technology of preparing of cost-effective graphene coating alumina-base material at present.
Summary of the invention
The object of the present invention is to provide a kind of new alumina-base material coating technologies.It is super by laser melting coating and high energy
Pre-made powder is sintered in surface of steel plate under the synergistic effect of sound, with the work of the corrosion resistance or the hardness that improve basis material etc.
Process.This method cladding layer controllability is high, customization is stronger, and using new method and proportion addition graphene oxide in matrix
Surface, at low cost, low failure rate.Graphene oxide has TiO due to surface2Coating has certain journey to graphene oxide under high temperature
Degree protection.Meanwhile silicon phase (Si) and graphene oxide generate micro SiC in situ, since it is generated for internal in-situ, thus boundary
Face cleaning binding performance is preferable.In addition, pool depth can be increased to a certain extent due to the effect of high-energy ultrasonic, enhancing is improved
The dispersibility of phase simultaneously improves wetting.
The present invention is achieved by the following technical solutions.
A kind of coated with titanium oxide of the present invention/graphene oxide surface of steel plate coating cladding ultrasonic method, including it is following
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 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.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, thin iron powder, fine silica powder, and glycerine is added,
Wherein silicon powder control is total powder quality 4 ~ 6.5%, and titanium valve control is the 4.5 ~ 7.5% of total powder quality, and size Control is 4 ~ 8 μ
M, the mass ratio of graphene oxide are 4 ~ 6%, and surplus is iron powder, and size Control is 3 ~ 12 μm.Glycerine be total volume ratio 3 ~
6%, this is crucial for stomata control, and then with 1 ~ 3h is ultrasonically treated, mixed powder process should keep preferable aridity, finally obtain glue
The mixed-powder of glutinous state.
(7) steel plate 1500 ~ 2000# sand paper is polished, alcohol washes drying.After will gluing state obtained by step (5) is mixed
It closes powder and is uniformly applied to steel surface, prefabricated thickness control is 0.4 ~ 1.3mm.Flame gun Quick uniform presintering powder is used again
In matrix surface.
(8) steel plate materials obtained by step (7) are put into argon gas guard box, steel plate, which should be fixed on bottom, among these high energy
It is fixed on the titanium alloy plate of ultrasound and with fixture.
(9) laser melting and coating technique is recycled to handle material.Its process parameter control are as follows: laser power should be controlled strictly
It is made as 0.9 ~ 1.5Kw, scanning speed is 5 ~ 7mm/s, and spot diameter is 2 ~ 4mm.In cladding process, high-energy ultrasonic collaboration is carried out,
Its power is controllably the interruption ultrasound under continual ultrasonic or 0.6Kw under 0.1 ~ 0.3Kw, and frequency is 20HZ ~ 10HZ transformation, transformation
Rate is that 0.5S is primary.
Hydrothermal reaction kettle liner described in step (3) of the present invention is polytetrafluoroethylene (PTFE).
The present invention has following uniqueness: (1) solution is using ethyl alcohol rather than water, participation reaction itself simultaneously increase volatilization
Property, pressure is bigger, beneficial to the surface tension for reducing solution.(2) in alcohol thermal response, prolonged low-temperature reduction can have the method
Effect abatement graphene oxide Guan Nengtuan extra after adsorbing metal ions.(3) this method is simple and effective is suitable for batch production.
(4) method introduces high-energy ultrasonic, can further improve the dispersion and wetability of graphene oxide.(5) in melt solidification
Ultrasound makes crystal grain become more uniform, and crystal boundary is more, can improve the hardness of material surface to a certain degree, increases wearability.
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.Wherein, glycerine and tetraisopropyl titanate volume ratio are 10:0.4.Hydro-thermal process is carried out later, wherein suspended
Liquid product accounts for the molten product 50% of reaction kettle.Place into reacting furnace and heat, 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, 10h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into point
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.It afterwards will be in gained powder under protection of argon gas 450 DEG C
Roasting.Time controls in 2h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.Gained powder is put
Enter in beaker, titanium valve, thin iron powder, fine silica powder is added, and glycerine is added, wherein silicon powder control is total powder quality 5%, titanium valve
Control is the 5.5% of total powder quality, and size Control is 7 μm, and the mass ratio of graphene oxide is 4%, and surplus is iron powder, size control
It is made as 5 μm.Glycerine is the 4% of total volume ratio, this is crucial for stomata control, handles whole process without steam, and then with ultrasonic treatment
2h.Obtain the mixed-powder of gluing state.
45# is polished in batches with 1500 ~ 2000 model sand paper, alcohol washes drying.Gained gluing state mixed-powder
It is uniformly applied to matrix surface, prefabricated thickness control is 0.7mm.Again with flame gun Quick uniform presintering powder in matrix table
Face.Material is handled using laser melting coating and high-energy ultrasonic in argon gas guard box later.Its process parameter control are as follows:
Laser power is 0.9Kw, and scanning speed 6mm/s, spot diameter is about 2mm.High-energy ultrasonic power 0.1Kw, is ground by data
Damage experiment has dropped nearly 17.5% it is found that the wear rate of coating is compared to matrix in load 200N.
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.Volume
Than being strict controlled in 0.2:50, after that gained dispersion liquid poured into sealing in the precursor liquid of glycerine and tetraisopropyl titanate composition is super
Sonication 1h.Wherein, glycerine and tetraisopropyl titanate volume ratio are 10:0.8.Hydro-thermal process is carried out later, wherein suspension
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/min
After being warming up to 180 DEG C, 12h 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 450 DEG C afterwards
It burns.Time controls in 1h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.Gained powder is put into burning
In cup, titanium valve, thin iron powder, fine silica powder is added, and glycerine is added, silicon powder control is total powder quality 6%, titanium valve control among these
It is made as the 6% of total powder quality, size Control is 4 μm, and the mass ratio of GO is 6%, and surplus is iron powder, and size Control is 8 μm.The third three
Alcohol is the 6% of total volume ratio, this is crucial for stomata control, handles whole process without steam, and then with ultrasonic treatment 3h.Obtain gluing
The mixed-powder of state.
Q375 is polished in batches with 1500 ~ 2000 model sand paper, alcohol washes drying.Gained gluing state mixed-powder
It is uniformly applied to matrix surface, prefabricated thickness control is 0.8mm.Again with flame gun Quick uniform presintering powder in matrix table
Face.Material is handled using laser melting coating and high-energy ultrasonic in argon gas guard box later.Its process parameter control are as follows:
Laser power is 1.0Kw, and scanning speed 7mm/s, spot diameter is about 3mm.High-energy ultrasonic power 0.3Kw, is ground by data
Damage experiment has dropped nearly 19% it is found that the wear rate of coating is compared to matrix in load 200N.It is compared to and does not lead
Enter ultrasound, hardness is greater than 12.7%.
Claims (1)
1. a kind of coated with titanium oxide/graphene oxide surface of steel plate coating cladding ultrasonic method, feature the following steps are included:
(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 are controlled in 9000 ~ 16000rpm；Whole process sealing guarantees 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, thin iron powder, fine silica powder, and glycerine is added, this its
Middle silicon powder control is total powder quality 4 ~ 6.5%, and titanium valve control is the 4.5 ~ 7.5% of total powder quality, and size Control is 4 ~ 8 μm,
The mass ratio of graphene oxide is 4 ~ 6%, and surplus is iron powder, and size Control is 3 ~ 12 μm；Glycerine is the 3 ~ 6% of total volume ratio,
This is crucial for stomata control, and then with 1 ~ 3h is ultrasonically treated, mixed powder process should keep drying, finally obtain the mixed powder of gluing state
End；
(7) steel plate 1500 ~ 2000# sand paper is polished, then alcohol washes drying will mix gluing state obtained by step (5)
Powder is uniformly applied to steel surface, and prefabricated thickness control is 0.4 ~ 1.3mm, then with flame gun Quick uniform presintering powder in
Matrix surface；
(8) steel plate materials obtained by step (7) are put into argon gas guard box, Interal fixation has the titanium alloy of high-energy ultrasonic in bottom
It is fixed on plate and with fixture；
(9) laser melting and coating technique is recycled to handle material, process parameter control are as follows: laser power answers the strict control to be
0.9 ~ 1.5kW, scanning speed are 5 ~ 7mm/s, and spot diameter is 2 ~ 4mm；In cladding process, high-energy ultrasonic collaboration is carried out, function
Rate is controllably the interruption ultrasound under continual ultrasonic or 0.6kW under 0.1 ~ 0.3kW, and frequency is 20Hz ~ 10Hz transformation, transformation
Rate is that 0.5s is primary；
Hydrothermal reaction kettle liner described in step (3) is polytetrafluoroethylene (PTFE).
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| CN110629130B (en) * | 2019-09-18 | 2020-08-14 | 北京石墨烯技术研究院有限公司 | Graphene oxide composite iron-based alloy powder, coating preparation method and product |
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 |
| 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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