CN115156004A - Preparation method of patterned gradient wetting functional surface with biocompatibility - Google Patents
Preparation method of patterned gradient wetting functional surface with biocompatibility Download PDFInfo
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- CN115156004A CN115156004A CN202210942724.2A CN202210942724A CN115156004A CN 115156004 A CN115156004 A CN 115156004A CN 202210942724 A CN202210942724 A CN 202210942724A CN 115156004 A CN115156004 A CN 115156004A
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- 238000000034 method Methods 0.000 claims abstract description 36
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- 238000005516 engineering process Methods 0.000 claims abstract description 7
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- 238000004132 cross linking Methods 0.000 claims abstract description 3
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- 238000003756 stirring Methods 0.000 claims description 28
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- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
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- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 3
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- CYUZOYPRAQASLN-UHFFFAOYSA-N 3-prop-2-enoyloxypropanoic acid Chemical compound OC(=O)CCOC(=O)C=C CYUZOYPRAQASLN-UHFFFAOYSA-N 0.000 claims description 3
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- 238000012545 processing Methods 0.000 claims description 2
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- ATZHWSYYKQKSSY-UHFFFAOYSA-N tetradecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)=C ATZHWSYYKQKSSY-UHFFFAOYSA-N 0.000 claims description 2
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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
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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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
- B05D3/002—Pretreatement
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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
- B05D3/02—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 baking
- B05D3/0254—After-treatment
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1802—C2-(meth)acrylate, e.g. ethyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/062—Copolymers with monomers not covered by C09D133/06
- C09D133/064—Copolymers with monomers not covered by C09D133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/062—Copolymers with monomers not covered by C09D133/06
- C09D133/066—Copolymers with monomers not covered by C09D133/06 containing -OH groups
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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
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- Chemical & Material Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention discloses a preparation method of a patterned gradient wetting functional surface with biocompatibility, which comprises the steps of preparing a metal surface with different microscopic patterns by a 3D metal laser sintering technology, then preparing a methacrylate resin solution, crosslinking with a curing agent, forming a compact polymer film on the metal surface with the different microscopic patterns, and adjusting the wetting time and the wetting concentration of an aqueous solution to form the patterned gradient wetting functional surface with biocompatibility and gradient change of a contact angle within a certain range. The functional surface prepared by the method has better biocompatibility and the characteristic of continuous change of gradient contact angles, can realize continuous and monotonous change of the contact angles in a larger range, enhances the protein adsorption capacity, can be realized on the surfaces of various metal materials, and greatly expands the application range of the gradient wetting functional surface in the protein adsorption capacity, specific adsorption behaviors and cell migration and growth processes.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a preparation method of a patterned gradient wetting functional surface with biocompatibility.
Background
Surface wettability has an important effect on protein adsorption, and different surface wettabilities can bring about different types of protein adsorption. The gradient wetting surface refers to the gradient continuous change of the contact angle of the surface of a material along a certain direction of the surface. Due to its unique properties, the gradient wetting surface has an important application in protein adsorption, which also puts higher demands on the biocompatibility of the gradient wetting functional surface material.
At present, the contact angle gradient continuity change of the surface is constructed on the surface of the biological material, and the surface chemical composition gradient change is mainly realized on the surface of the biological material. In the "Human serum albumin adsorption on to immunoglobulin based-silica gradient surface" article published by Hlady et al, colloids Surfaces B: biointerfaces (481-491, vol.2, 1994), octadecylsilane was used to form a gradient wetting surface with a gradient of surface chemical composition on a silicon wafer, to describe a gradient wetting surface with a surface contact angle increasing from 12 to 105, with the contact angle increasing, the adsorption of Human serum proteins increases, while the hydrophobic end of the gradient wetting surface exhibits better adsorption of immunoglobulins. In the "Combinatorial screen of the effect of surface energy on a graded surface addition, spraying and polishing" article published by Simon et al in Biomaterials (vol. 2006, 27, pages 3817-3824), a graded wetting surface with a gradient of surface energy was formed on a glass sheet using self-assembly of n-octyldimethylchlorosilane and UV illumination, describing that the growth of fibrin cells increases linearly with increasing contact angle and the growth rate is faster in the hydrophobic region on a graded wetting surface with increasing contact angle from 25 to 95.
The protein adsorption and cell adhesion on the gradient wetting surface are not only determined by the surface contact angle, but also influenced by the micro-topography of the gradient wetting surface. Another method for constructing the continuous change of the contact angle gradient of the surface of the biological material is to realize the gradient change of the microscopic topography of the surface of the biological material. The microtopography of the gradient wetting surface includes the patterning of the gradient wetting surface. There is currently less interest in patterning gradient wetted surfaces.
Disclosure of Invention
In view of the above technical problems, the present invention aims to provide a method for preparing a patterned gradient wetting functional surface with biocompatibility, which is simple and easy to operate.
Therefore, the invention provides a method for preparing a patterned gradient wetting functional surface with biocompatibility, which comprises the following steps:
(1) Preparing a metal surface with different microscopic patterns by a 3D metal laser sintering technology;
(2) Preparing a methacrylate resin solution, crosslinking with a curing agent, forming a compact polymer film on the metal surface in the step (1), adjusting the soaking time and the soaking concentration of the aqueous solution, and forming a patterned gradient wetting functional surface which has biocompatibility and the gradient change of a contact angle in a certain range.
Further, the preparation method of the step (2) specifically comprises the following steps:
(a) Adding 4-25 parts by mass of a first initiator and 80-450 parts by mass of a first monomer into a closed magnetic stirrer with the rotating speed of 20-90 revolutions per minute, and stirring for 8-25 minutes to obtain a first prepolymer monomer;
(b) Adding 4-25 parts of second initiator and 400-1200 parts of second monomer into a closed magnetic stirrer with the rotating speed of 20-90 revolutions per minute in parts by mass, and stirring for 8-35 minutes to obtain a second prepolymer monomer;
(c) Gradually dripping the first prepolymer monomer obtained in the step (a) into a four-neck flask containing 800-3600 parts of solvent and stirring at the speed of 200-450 revolutions per minute in parts by mass, finishing dripping within 15-70 minutes, gradually dripping the second prepolymer monomer obtained in the step (II) into the four-neck flask, finishing dripping within 15-70 minutes, and heating and stirring at 80-150 ℃ for 2-6 hours to obtain a polymer solution;
(d) Mixing the polymer solution obtained in the step (b) with 1-6 parts of curing agent by mass, adding the mixture into a closed magnetic stirrer with the rotating speed of 30-90 revolutions per minute, and stirring for 8-35 minutes to obtain a pre-curing solution;
(e) Uniformly coating the pre-curing solution obtained in the step (d) on the clean metal surface of the micro-pattern obtained in the step (1), and putting the clean metal surface into a drying oven at the temperature of 100-180 ℃ for heating and curing for 8-45 minutes to obtain a cured coating;
(f) Vertically placing the cured coating obtained in the step (e) in an open container, and gradually dropwise adding an aqueous solution into the container to ensure that the upper edge of the substrate is just completely soaked after dropwise adding is finished for 2-8 hours to obtain a pre-functional coating;
(g) And (f) placing the pre-functional coating obtained in the step (f) into distilled water for washing for 2-5 times, drying at the temperature of 30-60 ℃ after washing, and drying to finish the patterned gradient wetting functional surface with biocompatibility.
Preferably, the first initiator is one or more of azobisisobutyronitrile, benzoyl peroxide, acetyl peroxide, dodecanoyl peroxide and cumyl peroxide.
Preferably, the first monomer is one or more of hydroxyethyl methacrylate, hydroxypropyl methacrylate, carboxyethyl acrylate and hydroxypropyl acrylate.
Preferably, the second initiator is one or more of azobisisobutyronitrile, benzoyl peroxide, acetyl peroxide, dodecanoyl peroxide or cumene peroxide.
Preferably, the second monomer is one or more of methyl methacrylate, ethyl methacrylate, propyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, t-butyl methacrylate, tetradecyl methacrylate and octadecyl methacrylate.
Preferably, the solvent in (c) is one or more of toluene, xylene, butyl acetate and cyclohexane.
Preferably, the curing agent in (d) is amino resin or isocyanate.
Preferably, the aqueous solution in (f) is any one of a sodium hydroxide solution, a potassium hydroxide solution, a hydrochloric acid solution, a sulfuric acid solution, a phosphoric acid solution, or a benzoic acid solution at a concentration of 0.01mol/L to 10 mol/L.
Preferably, the microscopic pattern in step (1) includes one or more of a triangle, a quadrangle, a pentagon, a hexagon, a heptagon, and a hemisphere.
Preferably, in the step (1), the 3D metal laser sintering technology is implemented by a 3D metal printer, and the metal surface refers to one or more of an alloy surface, a silver surface, a copper surface, a cobalt-chromium alloy surface, a stainless steel surface, a nickel alloy surface, an aluminum alloy surface, and a titanium alloy surface.
Further, the 3D metal laser sintering technology in step (1) is used to prepare the metal surface in the following manner:
1) Firstly, a three-dimensional modeling software and a CAD workstation are utilized to create metal surface three-dimensional models with different wedge angles, and model three-dimensional data are obtained;
2) Processing the three-dimensional data: firstly, converting a data format from software into an STL data format suitable for generating a 3D printing process file; secondly, checking and analyzing errors of the STL data; then, estimating the consumption of printing consumables and the size of the sample according to the requirements of the metal sample; finally, editing the STL file and exporting a 3D printing process file;
3) The rapid prototyping equipment prints: and 3D metal laser sintering printing equipment is selected to complete the preparation of the wedge-shaped metal surface according to the characteristics of the metal sample material, the wedge-shaped angle requirement and the like.
The printer information is as follows: the manufacturer: TRUMPF SISMA S.r.I.Via Plemonte,4 36015SCHIO (VI) ITALY, model: g01, encoding: LS0008938.
Compared with the prior art, the invention has the beneficial effects that:
the functional surface prepared by the method has better biocompatibility, and the microscopic pattern characteristics of the functional surface can enhance the recognition of protein adsorption quantity, specific adsorption behavior and cell migration and growth processes; the prepared functional surface has the characteristic of continuous change of gradient contact angles, and can further promote the understanding of protein adsorption quantity, specific adsorption behavior and cell migration and growth processes on the surface with the continuous change of the contact angles; the continuous monotonous change of the contact angle within the range of 20 +/-10 degrees to 160 +/-10 degrees can be realized; the functional surface prepared by the method can be realized on the surfaces of materials such as an alloy surface, a silver surface, a copper surface, a cobalt-chromium alloy surface, a stainless steel surface, a nickel alloy surface, an aluminum alloy surface, a titanium alloy surface and the like, and the application range of the gradient wetting functional surface in the processes of protein adsorption capacity, specific adsorption behavior and cell migration and growth is greatly expanded.
Drawings
FIG. 1 is a surface view of a copper-based material having a triangularly arranged surface prepared by example 1 of the present invention;
FIG. 2 is a surface view of an aluminum alloy material having a quadrangular arrangement on the surface, prepared in example 2 of the present invention;
FIG. 3 is a surface view of a stainless steel material having pentagonal surface arrangement prepared in example 3 of the present invention;
FIG. 4 is a surface view of a titanium alloy material having a hexagonal arrangement on the surface prepared in example 4 of the present invention;
FIG. 5 is a surface view of a titanium alloy material having no hexagonal arrangement on the surface.
Detailed Description
The following further describes specific embodiments of the present disclosure with reference to the drawings, and these embodiments are intended to describe the present disclosure in detail, but not to limit the present disclosure. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present description.
Example 1
A method for preparing a patterned gradient wetting functional surface with biocompatibility, comprising the following steps:
the method comprises the steps of firstly, creating a three-dimensional model with different surface micro patterns and triangular arrangement of the copper-based surface by utilizing three-dimensional modeling software and a Computer-Aided Design (CAD) workstation, obtaining three-dimensional data of the model and a 3D printing process file, and selecting 3D metal laser sintering printing equipment to complete preparation of metal materials with triangular arrangement of the copper-based surface. The copper-based material model with triangularly arranged surfaces is shown in fig. 1.
Secondly, adding 16 g of azodiisobutyronitrile and 280 g of hydroxypropyl methacrylate into a closed magnetic stirrer with the rotating speed of 80 revolutions per minute in parts by mass, and stirring for 20 minutes to obtain a first prepolymer monomer;
thirdly, adding 16 g of azodiisobutyronitrile and 600 g of methyl methacrylate into a closed magnetic stirrer with the rotating speed of 80 revolutions per minute in parts by mass, and stirring for 18 minutes to obtain a second pre-polymerization monomer;
step four, gradually dripping the first prepolymer monomer obtained in the step one into a four-neck flask containing 2500 g of dimethylbenzene and stirring at the speed of 320 revolutions per minute in parts by mass, finishing dripping within 50 minutes, dripping the second prepolymer monomer obtained in the step three into the four-neck flask, finishing dripping within 50 minutes, heating at 120 ℃ and stirring for 6 hours to obtain a polymer solution;
fifthly, mixing the polymer solution obtained in the third step with 4 g of isocyanate in parts by mass, adding the mixture into a closed magnetic stirrer with the rotating speed of 80 revolutions per minute, and stirring for 20 minutes to obtain a pre-cured solution;
step five, uniformly coating the pre-curing solution obtained in the step four on the copper sheet with a clean surface obtained in the step one, and putting the copper sheet into a drying oven at the temperature of 110 ℃ for heating and curing for 40 minutes to obtain a cured coating;
sixthly, vertically placing the cured coating obtained in the fifth step into an open container, gradually dropwise adding a sodium hydroxide solution with the concentration of 0.04mol/L into the container, and completely soaking the upper edge of the substrate after 4 hours of dropwise adding to obtain a pre-functional coating;
and seventhly, putting the pre-functional coating obtained in the sixth step into distilled water for cleaning for 4 times, drying at 45 ℃ after cleaning, and finishing the preparation of the functional coating with the gradient contact angle after drying, wherein the contact angle is increased from 20 degrees with long soaking time to 150 degrees with short soaking time.
As a result: the feature surface increased the amount of bovine serum albumin adsorbed by 5% compared to the uncoated substrate surface.
Example 2
A method for preparing a patterned gradient wetting functional surface with biocompatibility, comprising the following steps:
the method comprises the steps of firstly, creating a three-dimensional model with different surface micro patterns and aluminum alloy surface quadrilateral arrangement by utilizing three-dimensional modeling software and a CAD (Computer-Aided Design) workstation, obtaining model three-dimensional data and a 3D printing process file, and selecting 3D metal laser sintering printing equipment to complete the preparation of metal materials with aluminum alloy surface quadrilateral arrangement. The aluminum alloy material model with the quadrilateral arrangement on the surface is shown in FIG. 2;
secondly, adding 14 g of benzoyl peroxide and 250 g of hydroxyethyl methacrylate into a closed magnetic stirrer with the rotating speed of 60 revolutions per minute in parts by mass, and stirring for 15 minutes to obtain a first prepolymer monomer;
thirdly, adding 8 g of benzoyl peroxide and 500 g of ethyl methacrylate into a closed magnetic stirrer with the rotating speed of 70 revolutions per minute in parts by mass, and stirring for 16 minutes to obtain a second prepolymer monomer;
step four, gradually dripping the first prepolymer monomer obtained in the step one into a four-neck flask containing 2200 g of butyl acetate and stirring at the speed of 300 revolutions per minute in parts by mass, finishing dripping within 40 minutes, dripping the second prepolymer monomer obtained in the step three into the four-neck flask, finishing dripping within 40 minutes, and heating and stirring at 110 ℃ for 4 hours to obtain a polymer solution;
fifthly, mixing the polymer solution obtained in the third step with 3 g of amino resin in parts by mass, adding the mixture into a closed magnetic stirrer with the rotating speed of 60 revolutions per minute, and stirring for 15 minutes to obtain a pre-cured solution;
step five, uniformly coating the pre-curing solution obtained in the step four on the surface of the aluminum alloy material with clean surface obtained in the step one, and putting the aluminum alloy material into a drying oven with the temperature of 100 ℃ for heating and curing for 20 minutes to obtain a cured coating;
sixthly, vertically placing the cured coating obtained in the fifth step into an open container, gradually dropwise adding a potassium hydroxide solution with the concentration of 0.02mol/L into the container, and completely soaking the upper edge of the substrate after 3 hours of dropwise adding to obtain a pre-functional coating;
and seventhly, putting the pre-functional coating obtained in the sixth step into distilled water for cleaning for 3 times, drying at 35 ℃, and finishing the preparation of the functional coating with the gradient contact angle after drying, wherein the contact angle is increased from 18 degrees with long soaking time to 140 degrees with short soaking time.
As a result: the feature surface increased the bovine serum albumin adsorption by 6% compared to the uncoated substrate surface.
Example 3
A method for preparing a patterned gradient wetting functional surface with biocompatibility, comprising the following steps:
the method comprises the steps of firstly, creating a three-dimensional model with different surface micro patterns and arranged on a stainless steel surface pentagon by utilizing three-dimensional modeling software and a CAD (Computer-Aided Design) workstation, obtaining three-dimensional data of the model and a 3D printing process file, and selecting 3D metal laser sintering printing equipment to finish the preparation of metal materials arranged on the stainless steel surface pentagon. The stainless steel material model with pentagonal arrangement on the surface is shown in figure 3;
secondly, adding 18 g of acetyl peroxide and 300 g of hydroxypropyl acrylate into a closed magnetic stirrer with the rotating speed of 90 revolutions per minute in parts by mass, and stirring for 22 minutes to obtain a first prepolymer monomer;
thirdly, adding 18 g of lauroyl peroxide and 700 g of n-butyl methacrylate into a closed magnetic stirrer with the rotating speed of 85 revolutions per minute in parts by mass, and stirring for 22 minutes to obtain a second prepolymer monomer;
step four, gradually dripping the first prepolymer monomer obtained in the step one into a four-neck flask containing 2800 g of toluene at a stirring speed of 350 revolutions per minute in parts by mass, finishing dripping within 60 minutes, dripping the second prepolymer monomer obtained in the step three into the four-neck flask, finishing dripping within 60 minutes, heating and stirring at 130 ℃ for 6 hours to obtain a polymer solution;
fifthly, mixing the polymer solution obtained in the third step with 5 g of amino resin in parts by mass, adding the mixture into a closed magnetic stirrer with the rotating speed of 90 revolutions per minute, and stirring for 35 minutes to obtain a pre-cured solution;
sixthly, uniformly coating the pre-curing solution obtained in the fourth step on the stainless steel material with a clean surface obtained in the first step, and heating and curing the stainless steel material in a drying oven at the temperature of 130 ℃ for 45 minutes to obtain a cured coating;
sixthly, vertically placing the cured coating obtained in the fifth step into an open container, gradually dropwise adding a hydrochloric acid solution with the concentration of 5mol/L into the container, and completely soaking the upper edge of the substrate after 7 hours of dropwise adding to obtain a pre-functional coating;
and seventhly, putting the pre-functional coating obtained in the sixth step into distilled water for cleaning for 5 times, drying at 55 ℃, and finishing the preparation of the functional coating with the gradient contact angle after drying, wherein the contact angle is increased from 20 degrees with long soaking time to 155 degrees with short soaking time.
The result is an increase in bovine serum albumin adsorption of 8% for the feature surface compared to the uncoated substrate surface.
Example 4
A method for preparing a patterned gradient wetting functional surface with biocompatibility, comprising the following steps:
the method comprises the steps of firstly, creating a three-dimensional model with different surface micro patterns and hexagonal arrangement on the surface of the titanium alloy by utilizing three-dimensional modeling software and a Computer-Aided Design (CAD) workstation, obtaining three-dimensional data of the model and a 3D printing process file, and selecting 3D metal laser sintering printing equipment to complete the preparation of metal materials with hexagonal arrangement and hemispherical arrangement on the surface of the titanium alloy. The titanium alloy material preparation model with the surface in hexagonal arrangement and hemispherical arrangement is shown in FIG. 4;
secondly, adding 17 g of acetyl peroxide and 320 g of carboxyethyl acrylate into a closed magnetic stirrer with the rotating speed of 90 revolutions per minute in parts by mass, and stirring for 24 minutes to obtain a first prepolymer monomer;
thirdly, adding 12 g of azodiisobutyronitrile and 500 g of isobutyl methacrylate into a closed magnetic stirrer at the rotating speed of 60 revolutions per minute in parts by mass, and stirring for 12 minutes to obtain a second pre-polymerization monomer;
fourthly, mixing the polymer solution obtained in the third step with 2.8 g of isocyanate in parts by mass, adding the mixture into a closed magnetic stirrer with the rotating speed of 50 revolutions per minute, and stirring for 10 minutes to obtain a pre-curing solution;
step five, uniformly coating the pre-curing solution obtained in the step four on the titanium alloy material with a clean surface obtained in the step one, and putting the titanium alloy material into a drying oven at 125 ℃ for heating and curing for 43 minutes to obtain a cured coating;
sixthly, vertically placing the cured coating obtained in the fifth step into an open container, gradually dropwise adding a potassium hydroxide solution with the concentration of 2mol/L into the container, and completely soaking the upper edge of the substrate after 2.2 hours of dropwise adding time to obtain a pre-functional coating;
and seventhly, putting the pre-functional coating obtained in the sixth step into distilled water for cleaning for 3 times, drying at 55 ℃, and finishing the preparation of the functional coating with the gradient contact angle after drying, wherein the contact angle of the surface hexagonally-arranged material is increased from 16 degrees with long soaking time to 130 degrees with short soaking time.
As a result: the feature surface increased the amount of bovine serum albumin adsorbed by 10% compared to the uncoated substrate surface.
Although the embodiments of the present description have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations may be made in these embodiments without departing from the principles and spirit of the description, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for preparing a patterned gradient wetting functional surface with biocompatibility, comprising the following steps:
(1) Preparing a metal surface with different microscopic patterns by a 3D metal laser sintering technology;
(2) Preparing a methacrylate resin solution, crosslinking with a curing agent, forming a compact polymer film on the metal surface in the step (1), adjusting the soaking time and the soaking concentration of the aqueous solution, and forming a patterned gradient wetting functional surface which has biocompatibility and the gradient change of a contact angle in a certain range.
2. The method for preparing a patterned gradient wetting functional surface with biocompatibility according to claim 1, wherein the preparation method of the step (2) is specifically as follows:
(a) Adding 4-25 parts by mass of a first initiator and 80-450 parts by mass of a first monomer into a closed magnetic stirrer with the rotating speed of 20-90 revolutions per minute, and stirring for 8-25 minutes to obtain a first prepolymer monomer;
(b) Adding 4-25 parts of second initiator and 400-1200 parts of second monomer into a closed magnetic stirrer with the rotating speed of 20-90 revolutions per minute in parts by mass, and stirring for 8-35 minutes to obtain a second prepolymer monomer;
(c) Gradually dripping the first prepolymer monomer obtained in the step (a) into a four-neck flask containing 800-3600 parts of solvent and stirring at the speed of 200-450 revolutions per minute in parts by mass, finishing dripping within 15-70 minutes, gradually dripping the second prepolymer monomer obtained in the step (II) into the four-neck flask, finishing dripping within 15-70 minutes, and heating and stirring at 80-150 ℃ for 2-6 hours to obtain a polymer solution;
(d) Mixing the polymer solution obtained in the step (b) with 1-6 parts of curing agent by mass part, adding the mixture into a closed magnetic stirrer with the rotating speed of 30-90 revolutions per minute, and stirring for 8-35 minutes to obtain a pre-curing solution;
(e) Uniformly coating the pre-curing solution obtained in the step (d) on the clean metal surface of the micro-pattern obtained in the step (1), and putting the clean metal surface into a drying oven at the temperature of 100-180 ℃ for heating and curing for 8-45 minutes to obtain a cured coating;
(f) Vertically placing the cured coating obtained in the step (e) in an open container, and gradually dropwise adding an aqueous solution into the container to ensure that the upper edge of the substrate is just completely soaked after dropwise adding is finished for 2-8 hours to obtain a pre-functional coating;
(g) And (f) placing the pre-functional coating obtained in the step (f) into distilled water for washing for 2-5 times, drying at the temperature of 30-60 ℃ after washing, and drying to finish the patterned gradient wetting functional surface with biocompatibility.
3. The method of claim 2, wherein the first initiator is one or more of azobisisobutyronitrile, benzoyl peroxide, acetyl peroxide, dodecanoyl peroxide and cumene peroxide; and/or the first monomer is one or more of hydroxyethyl methacrylate, hydroxypropyl methacrylate, carboxyethyl acrylate and hydroxypropyl acrylate.
4. The method of claim 2, wherein the second initiator is one or more of azobisisobutyronitrile, benzoyl peroxide, acetyl peroxide, dodecanoyl peroxide, or cumene peroxide; and/or the second monomer is one or more of methyl methacrylate, ethyl methacrylate, propyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, tert-butyl methacrylate, tetradecyl methacrylate and octadecyl methacrylate.
5. The method of claim 2, wherein the solvent in (c) is one or more of toluene, xylene, butyl acetate and cyclohexane.
6. The method of claim 2, wherein the curing agent in (d) is amino resin or isocyanate.
7. The method of claim 2, wherein the aqueous solution in (f) is any one of a sodium hydroxide solution, a potassium hydroxide solution, a hydrochloric acid solution, a sulfuric acid solution, a phosphoric acid solution, or a benzoic acid solution with a concentration of 0.01mol/L to 10 mol/L.
8. The method of claim 1, wherein the microscopic pattern of step (1) comprises one or more of a triangle, a quadrilateral, a pentagon, a hexagon, a heptagon and a hemisphere.
9. The method for preparing a patterned gradient wetting functional surface with biocompatibility according to claim 1, wherein in the step (1), the 3D metal laser sintering technology is implemented by a 3D metal printer, and the metal surface is one or more of a gold surface, a silver surface, a copper surface, a cobalt-chromium alloy surface, a stainless steel surface, a nickel alloy surface, an aluminum alloy surface, and a titanium alloy surface.
10. The method for preparing a patterned gradient wetting functional surface with biocompatibility according to claim 1, wherein the preparation of the metal surface by the 3D metal laser sintering technology in the step (1) is realized by the following steps:
1) Firstly, a three-dimensional modeling software and a CAD workstation are utilized to create metal surface three-dimensional models with different wedge angles, and model three-dimensional data are obtained;
2) Processing the three-dimensional data: firstly, converting a data format from software into an STL data format suitable for 3D printing process file generation; secondly, checking and analyzing errors of the STL data; then, estimating the consumption of printing consumables and the size of the sample according to the requirements of the metal sample; finally, editing the STL file and exporting a 3D printing process file;
3) The rapid prototyping equipment prints: and 3D metal laser sintering printing equipment is selected to complete the preparation of the wedge-shaped metal surface according to the characteristics of the metal sample material, the wedge-shaped angle requirement and the like.
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| CN102433053A (en) * | 2011-09-07 | 2012-05-02 | 华南理工大学 | Functional coating with gradient contact angle function and preparation method thereof |
| CN110434337A (en) * | 2019-08-23 | 2019-11-12 | 广州番禺职业技术学院 | A kind of 3D printing prepares the preparation method of bionic intelligence metal material surface |
| CN110694875A (en) * | 2019-11-15 | 2020-01-17 | 南京理工大学 | Method for obtaining super-hydrophobic surface of stepped layered structure |
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| CN102433053A (en) * | 2011-09-07 | 2012-05-02 | 华南理工大学 | Functional coating with gradient contact angle function and preparation method thereof |
| CN110434337A (en) * | 2019-08-23 | 2019-11-12 | 广州番禺职业技术学院 | A kind of 3D printing prepares the preparation method of bionic intelligence metal material surface |
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