CN110548174A - Preparation method and application of super-hydrophobic pyrolytic carbon surface - Google Patents
Preparation method and application of super-hydrophobic pyrolytic carbon surface Download PDFInfo
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- CN110548174A CN110548174A CN201910815359.7A CN201910815359A CN110548174A CN 110548174 A CN110548174 A CN 110548174A CN 201910815359 A CN201910815359 A CN 201910815359A CN 110548174 A CN110548174 A CN 110548174A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/08—Carbon ; Graphite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/20—Materials or treatment for tissue regeneration for reconstruction of the heart, e.g. heart valves
Abstract
The invention belongs to the technical field of surface modification, and particularly relates to a preparation method and application of a super-hydrophobic pyrolytic carbon surface. The preparation method comprises the following steps: (1) pretreatment: polishing, ultrasonically cleaning and drying the pyrolytic carbon sheet; (2) performing laser etching, ultrasonic cleaning and drying on the surface of the pyrolytic carbon sheet pretreated in the step (1) by using an infrared marking machine to obtain a pyrolytic carbon sheet with a microstructure on the surface; (3) and (3) coating hexadecyl trimethoxy silane on the surface of the pyrolytic carbon sheet with the microstructure in the step (2), drying, cleaning and drying to obtain the super-hydrophobic pyrolytic carbon surface. The super-hydrophobic pyrolytic carbon prepared by the method has excellent super-hydrophobic performance, low equipment price and short processing time, can be applied in large scale and is easy to realize industrial production.
Description
Technical Field
The invention belongs to the technical field of surface modification, and particularly relates to a preparation method and application of a super-hydrophobic pyrolytic carbon surface.
Background
replacement of prosthetic heart valves is one of the most effective methods for treating heart valve diseases in clinic, and pyrolytic carbon is the first choice material for manufacturing mechanical heart valves at present due to good biocompatibility and anticoagulation performance. It belongs to the laminar graphite carbon, and is similar to the structure of graphite. Graphite is a hexagonal planar carbon layer structure consisting of carbon atoms in a covalent bond manner. These carbon layers are stacked and have weak interlayer bonding force. Pyrolytic carbon is different from graphite in that its carbon layers are disordered and thus have folds and deformations, so that it has a relatively high breaking strength and a relatively low elastic modulus, and has considerably better wear and fatigue resistance properties than graphite. As a medical carbon material, compared with a metal material, pyrolytic carbon is a chemically inert material, so that the pyrolytic carbon has good biocompatibility and does not generate ions harmful to organisms in vivo. Of course, pyrolytic carbon also has good anti-coagulation properties and can be directly applied to the cardiovascular system, which is the most important reason for the popularity of pyrolytic carbon. However, the anticoagulant properties are still insufficient compared to native heart valves, and patients who replace pyrolytic carbon mechanical valves are prone to thromboembolism, necessitating lifelong anticoagulation therapy. It is important to find a new way to improve the blood compatibility.
Li et Al use ion beam to inject nitrogen ion on the surface of pyrolytic carbon, ZHANG et Al use ion beam enhanced deposition synthesis, non-equilibrium magnetron sputtering technology, plasma immersion ion injection and deposition technology to prepare TiO 2 film, TiO 2/TiN composite gradient film, TiN/Ti multilayer film transition layer on the surface of the material, experiments show that the modified material surface blood compatibility is improved significantly, BOLZ et Al use plasma enhanced chemical vapor deposition to deposit a-SiC H film, Krzysztof et Al use RF PACVD technology to cover nano crystal diamond on Ti 6 Al 4 V alloy surface, CHEN et Al use RF magnetron sputtering technology to synthesize Ta 5+ doped film 2 material, and use dynamic coagulation time measurement and platelet adhesion test to research the blood compatibility of the film, although all research materials can improve the mechanical valve surface compatibility by performing various treatments, the surface compatibility of the valve material is mostly a high-temperature stable TiO film, the local laser coating or film with low cost is very difficult to be prepared, and the local laser heating of the surface of the valve is very high-efficiency.
Disclosure of Invention
In order to overcome the defects of weak binding force and high cost of a surface coating in the prior art, the invention provides a method for preparing a super-hydrophobic pyrolytic carbon surface by using infrared laser, which overcomes the defects of high cost and insufficient binding force between the coating and a substrate in the prior art, and the prepared surface microstructure has good quality and stability.
the invention is realized by the following technical scheme:
A preparation method of a super-hydrophobic pyrolytic carbon surface comprises the following steps:
(1) Pretreatment: polishing, ultrasonically cleaning and drying the pyrolytic carbon sheet;
(2) Performing laser etching, ultrasonic cleaning and drying on the surface of the pyrolytic carbon sheet pretreated in the step (1) by using an infrared marking machine to obtain a pyrolytic carbon sheet with a microstructure on the surface;
(3) And (3) coating hexadecyl trimethoxy silane on the surface of the pyrolytic carbon sheet with the microstructure in the step (2), drying, cleaning and drying to obtain the super-hydrophobic pyrolytic carbon surface.
The uniform coating of the pyrolytic carbon surface is realized by a spin coater.
Further, the pyrolytic carbon sheet in the step (1) needs sample embedding treatment before polishing, and the method specifically comprises the following steps: the method comprises the steps of placing a pyrolytic carbon sheet at the bottom of a cold embedding mold, pouring mixed liquid of prepared acrylic powder and an acrylic curing agent, standing for 10-15min until the mixed liquid is solidified, directly polishing the pyrolytic carbon sheet to solve the problem of uneven polishing, and adopting a method of solidifying acrylic glue on one side of the pyrolytic carbon sheet to facilitate uniform polishing.
Further, the grinding in the step (1) is to grind the surface of the pyrolytic carbon sheet, and the pyrolytic carbon sheet is sequentially ground by 600#, 1000#, 3000#, 5000#, and 7000# sandpaper and polished by a polishing machine until the surface is smooth; the drying temperature is 80-110 ℃.
preferably, the parameters of the laser etching in the step (2) are as follows: the laser wavelength is 1064nm, the laser output power is 30W, and the laser frequency is 20 kHz.
preferably, the scanning speed of the laser in the laser etching process in the step (2) is 100-500mm/s, the single exposure time is 2-5ms, and the interval between adjacent scanning lines is 75-100 μm.
Preferably, the ultrasonic cleaning in the steps (1) and (2) is ultrasonic cleaning with deionized water and absolute ethyl alcohol sequentially at 40-60 ℃ for 25-30 min.
preferably, the cleaning in the step (3) is ultrasonic cleaning for 2-3min by adopting absolute ethyl alcohol at 40-70 ℃; the drying is carried out for 2h at the temperature of 70-80 ℃, and then the heat preservation is carried out for 1.5-2h at the temperature of 100-.
The invention also aims to provide application of the super-hydrophobic pyrolytic carbon surface prepared by the method in treating heart valve diseases.
The invention has the beneficial effects that:
(1) According to the invention, the microstructure is directly processed on the surface of the matrix pyrolytic carbon by infrared laser, and the surface of the matrix pyrolytic carbon is coated with hexadecyl trimethoxy silane to change the surface energy of the matrix pyrolytic carbon, so that the purposes of super hydrophobicity and improvement of blood compatibility are achieved, and the problem that the service life is influenced by poor binding force between the matrix and the coating in other methods is solved.
(2) Compared with a femtosecond laser marking machine, a picosecond laser marking machine or an ultraviolet laser marking machine in the prior art, the adopted infrared nanosecond laser marking machine is low in price, short in processing time, capable of being applied in a large scale and easy to realize industrial production; in addition, although the size of the grating-shaped microstructure made by the infrared nanosecond laser marking machine is larger, the surface energy of the microstructure is reduced by coating hexadecyl trimethoxy silane on the surface of the microstructure so as to achieve the purpose of superhydrophobicity, and the contact angles of the superhydrophobic surfaces prepared by the method are all larger than 150 degrees.
(3) the anhydrous ethanol and the hexadecyl trimethoxy silane used in the invention do not cause adverse effect on human bodies, do not cause damage to ecological environment, and accord with the principle of green production; compared with the prior art that the method of utilizing silane gas has the defect that the gas concentration is difficult to control and the surface energy of the surface of the substrate is difficult to control in the vacuum condition, the method of directly coating hexadecyl trimethoxy silane has the advantages of simplicity and convenience.
Drawings
FIG. 1 is a microscopic structure view of the superhydrophobic pyrolytic carbon surface prepared in example 1;
FIG. 2 is a schematic view showing a contact angle of the superhydrophobic pyrolytic carbon surface prepared in example 1;
FIG. 3 is a microscopic structure view of the superhydrophobic pyrolytic carbon surface prepared in example 2;
FIG. 4 is a schematic view showing a contact angle of the superhydrophobic pyrolytic carbon surface prepared in example 2;
FIG. 5 is a graph of dynamic clotting time for smooth pyrolytic carbon and superhydrophobic pyrolytic carbon prepared in example 2.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments and drawings, but is not limited thereto.
The acrylic powder and the acrylic curing agent used in the invention are purchased from Guangzhou Ultrainstrument metallographical laboratory instruments GmbH and named CAP1000 acrylic powder and named CAH1000 acrylic curing agent.
Example 1
(1) Pretreatment: placing a pyrolytic carbon sheet with the thickness of 20mm multiplied by 2mm in a cold embedding mold, uniformly mixing 0.6g of acrylic powder and 0.48g of acrylic curing agent, pouring the mixture into the cold embedding mold to solidify for about 12 minutes, carrying out sample embedding treatment, sequentially grinding the pyrolytic carbon sheet subjected to sample embedding through 600#, 1000#, 3000#, 5000#, and 7000# abrasive paper, polishing the pyrolytic carbon sheet by using a polishing machine, removing acrylic glue on one side of the ground pyrolytic carbon sheet, sequentially carrying out ultrasonic cleaning through deionized water and absolute ethyl alcohol, wherein the cleaning temperature is 55 ℃, the cleaning time is 30 minutes, and the drying condition is drying in a constant-temperature oven with the temperature of 80 ℃ for 10 minutes to obtain a pretreated pyrolytic carbon sheet;
(2) Laser etching: and (2) etching the microstructure on the surface of the pretreated pyrolytic carbon obtained in the step (1) by using an infrared laser marking machine, wherein the laser etching process parameters are as follows: etching a grating-shaped microstructure by using laser frequency of 20kHz, laser power of 30w, laser wavelength of 1064nm, scanning speed of 100mm/s, scanning interval of 100 microns, scanning times of 5 times and single exposure time of 4ms, then sequentially using deionized water and absolute ethyl alcohol for ultrasonic cleaning to remove slag, cleaning at 40 ℃, frequency of 36kHz and cleaning time of 30min, and drying after cleaning to obtain the microstructure pyrolytic carbon sheet;
(3) Surface modification: and (3) putting the micro-structure pyrolytic carbon sheet obtained in the step (3) into a spin coater, spin-coating hexadecyl trimethoxy silane on the surface of the sheet, then putting the sheet into a forced air drying oven for drying at a constant temperature of 80 ℃ for 2 hours, raising the temperature of the forced air drying oven to 110 ℃, preserving the heat for 1.5 hours, and finally ultrasonically cleaning the sheet for 2 minutes by using absolute ethyl alcohol to prepare the super-hydrophobic pyrolytic carbon surface.
The microstructure of the surface of the superhydrophobic pyrolytic carbon prepared by the example is shown in fig. 1, and the surface has a micron-scale grating structure.
The contact angle of the superhydrophobic pyrolytic carbon surface prepared by the example is shown in fig. 2, and the water contact angle is 152.12 degrees.
Example 2
(1) Pretreatment: placing a pyrolytic carbon sheet with the thickness of 20mm multiplied by 2mm in a cold embedding mold, uniformly mixing 0.6g of acrylic powder and 0.48g of acrylic curing agent, pouring the mixture into the cold embedding mold to solidify for about 12 minutes, carrying out sample embedding treatment, sequentially grinding the pyrolytic carbon sheet subjected to sample embedding through 600#, 1000#, 3000#, 5000#, and 7000# abrasive paper, polishing the pyrolytic carbon sheet by using a polishing machine, removing acrylic glue on one side of the ground pyrolytic carbon sheet, sequentially carrying out ultrasonic cleaning through deionized water and absolute ethyl alcohol, wherein the cleaning temperature is 55 ℃, the cleaning time is 30 minutes, and the drying condition is drying in a constant-temperature oven with the temperature of 80 ℃ for 10 minutes to obtain a pretreated pyrolytic carbon sheet;
(2) Laser etching: and (2) etching the microstructure on the surface of the pretreated pyrolytic carbon obtained in the step (1) by using an infrared laser marking machine, wherein the laser etching process parameters are as follows: etching a grating-shaped microstructure by using laser frequency of 20kHz, laser power of 27.5W, laser wavelength of 1064nm, scanning speed of 100mm/s, scanning interval of 110 microns, scanning times of 5 times and single exposure time of 4ms, then sequentially performing ultrasonic cleaning by using deionized water and absolute ethyl alcohol to remove slag, cleaning at 40 ℃, frequency of 36kHz and cleaning time of 30min, and drying after cleaning to obtain a microstructure pyrolytic carbon sheet;
(3) Surface modification: and (3) putting the micro-structure pyrolytic carbon sheet obtained in the step (3) into a spin coater, spin-coating hexadecyl trimethoxy silane on the surface of the sheet, then putting the sheet into a forced air drying oven for drying at a constant temperature of 80 ℃ for 2 hours, raising the temperature of the forced air drying oven to 100 ℃, preserving the temperature for 2 hours, and finally ultrasonically cleaning the sheet for 2 minutes by using absolute ethyl alcohol to prepare the super-hydrophobic pyrolytic carbon surface.
The microstructure of the surface of the superhydrophobic pyrolytic carbon prepared by the example is shown in fig. 3, and the surface has a micron-scale grating structure.
The contact angle of the superhydrophobic pyrolytic carbon surface prepared by the example is shown in fig. 4, and the water contact angle is 153.84 degrees.
The prepared super-hydrophobic surface has regular appearance and higher water contact angles of 152.12 degrees and 153.84 degrees respectively. The specific etching parameter method has good effect on preparing the surface of the super-hydrophobic pyrolytic carbon.
Blood compatibility test:
polished smooth pyrolytic carbon (control group) and the superhydrophobic pyrolytic carbon (test group) prepared in example 2 are respectively placed at the bottom of a beaker, after the temperature is kept constant for 5min at 37 ℃, 0.25mL of anticoagulated rabbit blood (the anticoagulated rabbit blood is prepared according to the mass ratio of 7:1 of rabbit blood to anticoagulant, wherein the anticoagulant is prepared by adding 30g of sodium citrate, 10g of citric acid and 25g of glucose into distilled water to fix the volume to 1L) is injected into the center of a sample by using a microsyringe, after the temperature is kept constant for 5min, 0.02mL of CaCl 2 aqueous solution with the concentration of 0.2mol/L is injected into the blood, after the blood is uniformly stirred by using the microsyringe, the sample is kept still for a period of time (6 time points are adopted in the test, and are respectively represented by 10, 20, 30, 40, 50 and 60min), 25mL of distilled water is then added into the beaker, red blood cells which are not solidified on the sample are subjected to hemolysis, free hemoglobin is uniformly dispersed in water, and the concentration of the hemoglobin dissolved in the water is measured by using a spectrophotometer (absorbance at 540 nm).
fig. 5 is a dynamic coagulation time curve of smooth pyrolytic carbon and super-hydrophobic pyrolytic carbon, and it can be seen that, compared with smooth pyrolytic carbon, the anticoagulant performance of the super-hydrophobic pyrolytic carbon surface prepared in example 2 is obviously improved, which indicates that the super-hydrophobic pyrolytic carbon surface prepared by the method of the present invention has good blood compatibility.
Various other modifications and changes may be made by those skilled in the art based on the above-described technical solutions and concepts, and all such modifications and changes should fall within the scope of the claims of the present invention.
Claims (8)
1. A preparation method of a super-hydrophobic pyrolytic carbon surface is characterized by comprising the following steps:
(1) Pretreatment: polishing, ultrasonically cleaning and drying the pyrolytic carbon sheet;
(2) performing laser etching, ultrasonic cleaning and drying on the surface of the pyrolytic carbon sheet pretreated in the step (1) by using an infrared marking machine to obtain a pyrolytic carbon sheet with a microstructure on the surface;
(3) and (3) coating hexadecyl trimethoxy silane on the surface of the pyrolytic carbon sheet with the microstructure in the step (2), drying, cleaning and drying to obtain the super-hydrophobic pyrolytic carbon surface.
2. The method for preparing the superhydrophobic pyrolytic carbon surface according to claim 1, wherein the pyrolytic carbon sheet in step (1) needs to be subjected to sample embedding treatment before being polished, specifically: and (3) placing the pyrolytic carbon sheet at the bottom of the cold embedding mold, then pouring the prepared mixed solution of the acrylic powder and the acrylic curing agent, and standing for 10-15min until the mixed solution is solidified.
3. The method for preparing the superhydrophobic pyrolytic carbon surface according to claim 1, wherein the grinding in step (1) is to grind the surface of a pyrolytic carbon sheet, sequentially grind through 600#, 1000#, 3000#, 5000#, 7000# sandpaper and polish the surface to be smooth through a polishing machine; the drying temperature is 80-110 ℃.
4. The method for preparing the superhydrophobic pyrolytic carbon surface according to claim 1, wherein the parameters of the laser etching in the step (2) are as follows: the laser wavelength is 1064nm, the laser output power is 30W, and the laser frequency is 20 kHz.
5. the method as claimed in claim 1, wherein the scanning speed of the laser in the laser etching process in step (2) is 100-500mm/s, the single exposure time is 2-5ms, and the interval between adjacent scanning lines is 75-100 μm.
6. The method for preparing a superhydrophobic pyrolytic carbon surface according to claim 1, wherein the ultrasonic cleaning in steps (1) and (2) is ultrasonic cleaning with deionized water and absolute ethanol sequentially at 40-60 ℃ for 25-30 min.
7. The method for preparing a superhydrophobic pyrolytic carbon surface according to claim 1, wherein the cleaning in step (3) is ultrasonic cleaning with absolute ethanol at 40-70 ℃ for 2-3 min; the drying is carried out for 2h at the temperature of 70-80 ℃, and then the heat preservation is carried out for 1.5-2h at the temperature of 100-.
8. Use of a superhydrophobic pyrolytic carbon surface prepared according to the method of any one of claims 1-7 in the treatment of heart valve disease.
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Cited By (2)
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| CN112775561A (en) * | 2020-12-31 | 2021-05-11 | 华东交通大学 | Pyrolytic carbon mechanical valve leaflet with two-stage pattern on surface and preparation method thereof |
| CN115008018A (en) * | 2022-04-28 | 2022-09-06 | 西安交通大学 | Method for preparing durable super-hydrophobic surface through femtosecond laser composite rare earth nano modification |
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