CN109465170A - The coating and its preparation method and application of light healing is fast implemented under a kind of response based on near-infrared laser - Google Patents
The coating and its preparation method and application of light healing is fast implemented under a kind of response based on near-infrared laser Download PDFInfo
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- CN109465170A CN109465170A CN201811120922.0A CN201811120922A CN109465170A CN 109465170 A CN109465170 A CN 109465170A CN 201811120922 A CN201811120922 A CN 201811120922A CN 109465170 A CN109465170 A CN 109465170A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0406—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
- B05D3/0426—Cooling with air
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/102—Pretreatment of metallic substrates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/105—Intermediate treatments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/51—One specific pretreatment, e.g. phosphatation, chromatation, in combination with one specific coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/56—Three layers or more
- B05D7/58—No clear coat specified
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F15/00—Other methods of preventing corrosion or incrustation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2508/00—Polyesters
Abstract
It is a kind of based on near-infrared laser response under fast implement light healing coating preparation method, include the following steps: S1, dried up using magnesium metal disk as substrate, and after ultrasound it is spare;S2, the magnesium alloy substrate cleaned by step S1 is immersed in hydrofluoric acid, Mg alloy surface is made to form one layer of MgF2Pretreatment coating;S3, in the uniform three strata caprolactone of spin coating of pretreated Mg alloy surface;S4, the magnesium alloy for handling S3 immerse in deionized water, then pyrroles, Fe(NO3)39H2O are successively added dropwise, so that Mg alloy surface forms one layer of black polypyrrole coating;S5, the Mg alloy surface spin coating polycaprolactone handled in S4 form one layer of polymeric coating layer with shape memory.Its advantage is that: the photo-thermal effect having using polypyrrole, under the irradiation of 808nm near-infrared laser, can be rapidly heated to required for polycaprolactone compared with low melting point temperature so that polycaprolactone play shape memory characteristic, quick non-union defect position achievees the purpose that delay corrosion process.
Description
Technical field
The present invention relates to the applied technical field of optothermal material and biological medical polymer material, specifically a kind of base
The coating and its preparation method and application of light healing is fast implemented under near-infrared laser response.
Background technique
In recent years, magnesium-base metal is repaired due to its excellent mechanical property and the degradability in physiological environment in tissue
Concern in terms of multiple and joint, structural transplantation by more and more researchers.Magnesium alloy can overcome titanium alloy, stainless steel and cobalt
The shortcomings that alloy cannot degrade in physiological environment and must receive second operation.But magnesium metal is active metal, in vivo
Degradation speed it is too fast, cause magnesium metal to lose the mechanical property close with natural bone too early, and in degradation process, produce
Alkalization is crossed in raw hydrogen and part will affect the growth of surrounding tissue cells, influence healing process be also possible to cause inflammation or its
The symptom of his discomfort.
Prepared on magnesium alloy intelligent stimuli responsive self-healing coating be it is a kind of prevent the too fast degradation of magnesium alloy it is effective
Method.Extraneous stimulation such as pH, redox reaction and Mg2+Deng, using oversubscription sub switch, such as Subjective and Objective reciprocation,
Redox reaction etc., the nano container of stimulation encapsulation in the coating discharges anticorrosive, or promotes to be formed in coating surface
Hydroxyapatite delays corrosion process.But these stimulating courses are slow, and preparation process is more complicated, it is time-consuming
Long.
Summary of the invention
The object of the present invention is to provide coatings and its system that light healing is fast implemented under a kind of response based on near-infrared laser
Preparation Method and application, to prepare while have the coating of light healing properties, good corrosion energy.
First aspect present invention protects a kind of preparation side that light healing coating is fast implemented under responding based on near-infrared laser
Method includes the following steps:
S1, dried up using magnesium metal disk as substrate, and after ultrasound it is spare;
S2, the magnesium alloy substrate cleaned by step S1 is immersed in hydrofluoric acid, Mg alloy surface is made to form one layer of MgF2
Pretreatment coating;
S3, in the uniform three strata caprolactone of spin coating of pretreated Mg alloy surface;
S4, the magnesium alloy for handling S3 immerse in deionized water, then pyrrole monomer, nine nitric hydrates are successively added dropwise
Iron, so that Mg alloy surface forms one layer of black polypyrrole coating;
S5, the 10 strata caprolactone of Mg alloy surface spin coating handled in S4 form one layer of macromolecule with shape memory
Coating.
Preferably, in step S1, magnesium metal disk uses sand paper step by step after surface polishing as substrate;
In step S1, the successively ultrasound 20min in ethyl alcohol, acetone by substrate, then cold wind drying are spare.
Preferably, in step S2, magnesium alloy substrate is immersed in the hydrofluoric acid of wt% >=40% three days.
Preferably, in step S3, three strata caprolactone of spin coating gathers in oneself to ensure that Mg alloy surface can cover
Ester, and three layers provide pre- protective effect enough for substrate.If two layers of spin coating is less, the heavy of polypyrrole coating is easily influenced
Long-pending and uniformity;If spin coating number is excessive, coating is too thick, and preparation process is cumbersome, wastes time;
Step S3, in S5, the revolving speed of spin coating is both preferably 5000rpm 30s, and the concentration of polycaprolactone is 80mg/
ML, 5000rpm high speed spin coating 30s are the too low homogeneity for being unfavorable for film of revolving speed and film in order to guarantee that the thickness of film is uniformly unified
It can thicken, the excessively high thickness that can make film of revolving speed is thinning, to influence subsequent smooth healing time;
Pyrrole monomer in step S4, in every 1ml deionized water containing 0.02g Fe(NO3)39H2O and 3ul.Nine hydrations
Ferric nitrate makes oxidizable pyrrole be polymerized to polypyrrole as oxidant, and in ratio as shown above, the amount of Fe(NO3)39H2O is enough
So that oxidizable pyrrole is polymerized to polypyrrole, if the amount of Fe(NO3)39H2O is on the low side, is unfavorable for pyrroles's complete oxidation;If nine water
The amount for closing ferric nitrate is on the high side, and since Fe(NO3)39H2O is hydrolyzed in aqueous solution in acidity, amount excessively reinforces solution acidic, base
Bottom may be corroded, and be unfavorable for pyrroles and be deposited in substrate;
In step S4, after Fe(NO3)39H2O and pyrrole monomer is added, reaction is maintained under the conditions of 4~6 DEG C and stands 2h,
Low temperature be maintained at 4~6 DEG C be oxidizable pyrrole aggregate into polypyrrole optimum temperature and reaction speed it is fast, save experimental period, protect
Card reaction carries out at a suitable temperature;
In step S5, the thickness of 10 strata caprolactones is about 125 microns.If 9 layers of spin coating is less, illumination makes coating
The time of upper scratch healing extends, and will increase phototoxicity;If spin coating number is excessive, coating is too thick, be not suitable for investment application and
It wastes raw material, so 10 layers are optimum spin coating numbers.
Light is fast implemented under the near-infrared laser response of second aspect of the present invention protection first aspect the method preparation to be cured
The material of conjunction.
Third aspect present invention protects application of the material on magnesium alloy anticorrosion material described in second aspect.
The coating and its preparation method and application of light healing, advantage are fast implemented under a kind of response based on near-infrared laser
It is:
The good photo-thermal effect having using polypyrrole (polypyrrole, PPy) shines in 808nm near-infrared laser
Penetrate down, can be rapidly heated to required for polycaprolactone (Polycaprolactone, PCL) compared with low melting point temperature so that poly-
Caprolactone plays the characteristic of shape memory, and quick non-union defect position achievees the purpose that delay corrosion process;
The figure layer even compact of the method for the present invention preparation, there is good Corrosion Protection;And it can be applied to magnesium alloy anti-corrosion
On corrosion material;Meanwhile this method equipment investment is few, consumption resource is few, highly-safe.
Detailed description of the invention
Fig. 1 is the surface topography map after prepared by embodiment 1;
Fig. 2 is the electrochemistry Tafel polarization curve of gained sample in embodiment 1,2,3;
Fig. 3 is the electrochemistry Ta Feier polarization of gained sample in embodiment 1,2,3 after impregnating one day in simulated body fluid
Curve;
Fig. 4 is the electrochemistry Ta Feier polarization of gained sample in embodiment 1,2,3 after impregnating seven days in simulated body fluid
Curve;
Fig. 5 is that gained sample carries out the surface after electro-chemical test in embodiment 1 after impregnating one day in simulated body fluid
Shape appearance figure;
Fig. 6 is that gained sample carries out the surface after electro-chemical test in embodiment 2 after impregnating one day in simulated body fluid
Shape appearance figure;
Fig. 7 is that gained sample carries out the surface after electro-chemical test in embodiment 3 after impregnating one day in simulated body fluid
Shape appearance figure;
Fig. 8 is that gained sample carries out the surface after electro-chemical test in embodiment 1 after impregnating seven days in simulated body fluid
Shape appearance figure;
Fig. 9 is that gained sample carries out the surface after electro-chemical test in embodiment 2 after impregnating seven days in simulated body fluid
Shape appearance figure;
Figure 10 is that gained sample carries out the surface after electro-chemical test in embodiment 3 after impregnating seven days in simulated body fluid
Shape appearance figure.
Specific embodiment
To be best understood from the present invention, the present invention is done further be described in detail with reference to the accompanying drawings and examples, still
The scope of protection of present invention is not limited to the range of embodiment expression.
Embodiment one
S1. by magnesium metal disk with being polishing to smooth mirror surface on polishing machine with the sand paper of different size respectively, then by its
The successively ultrasound 20min in ethyl alcohol, acetone, the pollutant on the clean surface of ultrasound, then cold wind drying is spare;
S2. the magnesium alloy substrate cleaned by step S1 is immersed in the hydrofluoric acid of wt% >=40% three days, makes magnesium alloy
Surface forms one layer of MgF2Pretreatment coating;
S3. in the uniform high speed three strata caprolactone of (5000rpm 30s) spin coating of pretreated Mg alloy surface, spin coating is three times
Ensure that Mg alloy surface can cover polycaprolactone, and three layers provide pre- protective effect enough for substrate.If spin coating two
Layer is less, will affect the deposition and uniformity of polypyrrole coating;If spin coating number is excessive, coating is too thick, prepares
Journey is cumbersome, wastes time.5000rpm high speed spin coating 30s is that revolving speed is too low to be unfavorable for film in order to guarantee that the thickness of film is uniformly unified
Homogeneity and film can thicken, the excessively high thickness that can make film of revolving speed is thinning, to influence subsequent smooth healing time,;
S4. magnesium alloy S3 handled immerses in 20mL deionized water, then be successively added dropwise 60 μ L pyrrole monomer,
Reaction is maintained at 4 DEG C and stands 2h by 0.4g Fe(NO3)39H2O, and Mg alloy surface will form the black of one layer of even compact
Polypyrrole coating;
S5. in the Mg alloy surface high speed 10 strata caprolactone of (5000rpm 30s) spin coating of S4 processing, forming one layer has
The polymeric coating layer of shape memory.Form MgF2The composite coating of/PCL/PPy/PCL.The thickness of 10 strata caprolactones is general
It is 125 microns.If 9 layers of spin coating is less, illumination extends the time that scratch heals on coating, may will increase light poison
Property;If spin coating number is excessive, coating is too thick, is not suitable for investment application and wastes raw material, so 10 layers are optimum rotations
Apply number.5000rpm high speed spin coating 30s is the too low homogeneity for being unfavorable for film of revolving speed in order to guarantee that the thickness of film is uniformly unified
And film can thicken, the excessively high thickness that can make film of revolving speed is thinning, so that light healing time is influenced,.
S6. apply one of scratch in the length, the width that in the sample coatings handled through S5, guarantee the scratch of same sample
Degree, depth are the same.The MgF with scratch is formed in substrate surface2The composite coating of/PCL/PPy/PCL.
S7. the sample handled through S6, which is placed under 808nm near infrared light, irradiates 6min.Light healing is formed in substrate surface
MgF2The composite coating of/PCL/PPy/PCL.
In the above-mentioned constant situation of other conditions, the product that will be obtained by step S1, S2, S5, S6, S7, using electrochemistry work
It stands and their impedance is tested;
Its test condition is that interference voltage is 10mV, range of scanned frequencies 10-2Hz-105Hz, acquired results are used
3.21 software of Zsimpwin is fitted:
The electrochemical impedance of magnesium alloy after fluorination treatment is hindered compared to the electrochemistry for the magnesium alloy not being modified
It is anti-to slightly increase;
By MgF2The magnesium sheet of/PCL/PPy/PCL coating modification is compared to the magnesium sheet not being modified, and electrochemical impedance value is substantially
Degree increases, and the Magnesium Anti-Corrosion after illustrating modification increases substantially, which can significantly improve the anticorrosion of magnesium alloy
Performance (as shown in Figure 2);
Apply the MgF after scratch simultaneously2/ PCL/PPy/PCL coating, electrochemical impedance value decrease speed are cured compared to light
MgF after conjunction2The decrease speed of/PCL/PPy/PCL faster, illustrates that near infrared light can make local scratch area heal, mentions
High anticorrosive property energy (as shown in Figure 2).
Embodiment two
With embodiment one the difference is that:
The obtained sample of step S5, S6, S7 is soaked in simulated body fluid respectively, and is kept for one day.Simulated body fluid
Initial pH value is 7.4, and keeps the temperature of soaking process at 37 degrees Celsius.It is i.e. complete, with scratch, light healing
MgF2The composite coating of/PCL/PPy/PCL is soaked in simulated body fluid, and is kept for one day.
Embodiment three
With embodiment one the difference is that: the obtained sample of step S5, S6, S7 is soaked in simulated body fluid respectively,
And it is kept for seven days.The initial pH value of simulated body fluid is 7.4, and keeps the temperature of soaking process at 37 degrees Celsius.It is i.e. complete
, the MgF of with scratch, light healing2The composite coating of/PCL/PPy/PCL is soaked in simulated body fluid, and keeps seven
It.
Electro-chemical test has been carried out to the impedance of the sample in embodiment one, two, three using electrochemical workstation:
Its test condition is that interference voltage is 10mV, range of scanned frequencies 10-2Hz-105Hz, acquired results are used
3.21 software of Zsimpwin is fitted:
Known to electrochemistry Tafel polarization curve (as shown in Figure 3), increase to one day with number of days is impregnated, corrosion current
It is all gradually increased, and keeps such trend; MgF2/ PCL/PPy/PCL scratch ﹥ MgF2/ PCL/PPy/PCL light healing ﹥
MgF2/PCL/PPy/PCL;
By electrochemistry Tafel polarization curve it is found that increasing to seven days (as shown in Figure 4) with number of days is impregnated, three groups of samples
The corrosion current of product is all gradually increased, and keeps such trend; MgF2/ PCL/PPy/PCL scratch ﹥ MgF2/PCL/PPy/PCL
Light healing ﹥ MgF2/PCL/PPy/PCL。
In soaking process, apply the MgF after scratch2/ PCL/PPy/PCL coating, electrochemical impedance value decrease speed
Compared to the MgF after light healing2The decrease speed of/PCL/PPy/PCL faster, illustrates near infrared light with can making local scratch
Area's healing, improves Corrosion Protection.
Surface shape of the sample in embodiment one, three after electro-chemical test is characterized by scanning electron microscope
Looks:
It is obtained by Fig. 1 observable, the surface topography that example one prepares is smooth, does not have defect;
By Fig. 5,6,7 it can be concluded that, after electro-chemical test, light healing after MgF2/ PCL/PPy/PCL is applied
Layer compares MgF2The spot corrosion that/PCL/PPy/PCL coating occurs is more, applies the MgF after scratch2/ PCL/PPy/PCL coating occurs
Spot corrosion is also relatively more, and spot corrosion area is bigger.
By Fig. 8,9,10, it can be concluded that, three groups of samples carry out electro-chemical test after impregnating seven days by simulated body fluid again,
MgF after light healing2/ PCL/PPy/PCL coating ratio MgF2/ PCL/PPy/PCL coating corrosion is more serious, and there is crackle production on surface
Raw, spot corrosion is more serious;Apply the MgF after scratch2/ PCL/PPy/PCL coating corrodes more serious at scratch, and surface has very
Multiple cracks generate.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. fast implementing the preparation method of light healing coating under a kind of response based on near-infrared laser, it is characterised in that: including such as
Lower step
S1, dried up using magnesium metal disk as substrate, and after ultrasound it is spare;
S2, the magnesium alloy substrate cleaned by step S1 is immersed in hydrofluoric acid, Mg alloy surface is made to form one layer of MgF2Pre- place
Manage coating;
S3, in the uniform three strata caprolactone of spin coating of pretreated Mg alloy surface;
After S4, the magnesium alloy for handling S3 immerse deionized water, then successively dropwise addition pyrrole monomer, Fe(NO3)39H2O make
Mg alloy surface forms one layer of black polypyrrole coating;
S5, the 10 strata caprolactone of Mg alloy surface spin coating handled in S4 form one layer of polymeric coating layer with shape memory.
2. method according to claim 1, it is characterised in that: in step S2, magnesium alloy substrate is immersed in wt% >=40%
Three days in hydrofluoric acid.
3. method according to claim 1, it is characterised in that: step S3, in S5, the revolving speed of spin coating is both preferably 5000rpm
30s, the concentration of polycaprolactone are 80mg/mL.
4. method according to claim 1, it is characterised in that: in step S4, nine water of 0.02g is contained in every 1ml deionized water
Close the pyrrole monomer of ferric nitrate and 3ul.
5. using the material for fast implementing light healing under the near-infrared laser response of Claims 1-4 the method preparation.
6. application of the material described in claim 5 on magnesium alloy anticorrosion material.
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