CN107823707B - Preparation method of honeycomb-shaped ordered porous graphene coating - Google Patents
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 8
- 238000001338 self-assembly Methods 0.000 claims abstract description 8
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- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 3
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- 239000000463 material Substances 0.000 abstract description 12
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- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 abstract 1
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- WAIPAZQMEIHHTJ-UHFFFAOYSA-N [Cr].[Co] Chemical class [Cr].[Co] WAIPAZQMEIHHTJ-UHFFFAOYSA-N 0.000 description 1
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- 229940088710 antibiotic agent Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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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
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
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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
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
-
- 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
- A61L27/56—Porous materials, e.g. foams or sponges
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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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
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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
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a preparation method of a honeycomb-shaped ordered porous graphene coating. The BreathFigure self-assembly ordered porous structure requires that materials are dissolved in an organic solvent, GO is strong in hydrophilicity but low in dispersibility in the organic solvent, GO can be transferred from a water phase to organic solvent phases such as chloroform and the like by utilizing the electrostatic interaction of a cationic surfactant such as dioctadecyl amine and GO, after the pretreatment such as cleaning of a Ti substrate and the like, a BreathFigure self-assembly method is adopted to prepare a honeycomb-shaped porous GO layer on the Ti substrate. And reducing the porous GO layer by using a reducing agent such as hydrazine hydrate or ascorbic acid to obtain the porous graphene layer. According to the invention, the honeycomb-shaped ordered porous graphene coating is prepared on the surface of the titanium material, and the prepared coating not only can provide antibacterial property, but also can regulate and control the function of osteoblasts and promote the rapid osseointegration of the bone-titanium material.
Description
Technical Field
The invention belongs to the technical field of medicine, and particularly relates to a preparation method of a honeycomb-shaped ordered porous graphene coating.
Background
The biomedical material can diagnose, treat, replace damaged tissues and organs or enhance the functions of the damaged tissues and organs of organisms, belongs to the field of medical instruments, is a cross marginal subject between biology, medicine, materials science and chemistry in research, almost covers the whole field of material science and life science, and has the characteristics of knowledge, technical density and cross of multiple subjects.
The history of biomedical research and development of titanium alloys dates back to the early 40 s of the 20 th century, and the Bothe et al first introduced pure titanium into the biomedical field, and they found that there was no adverse reaction between titanium and rat femur. After 10 years Leventhal further studies confirmed the good biocompatibility of pure titanium. However, since medical stainless steel and cobalt-chromium alloy have become prevalent during world war ii, titanium alloy has been applied and developed slowly in biomedical fields. Since the 60's Branemark used pure titanium for oral implants, pure titanium was widely developed as a surgical implant material, and the alpha titanium alloy Ti3Al2 · 5V was also used clinically as a femoral and tibial replacement material.
The surface of the medical titanium alloy implant material is lack of antibacterial property, so that the infection problem caused by bacterial adhesion is easy to occur. In the aspect of surface anti-infection of titanium alloy implant materials, antibacterial coatings are mostly adopted for modification, but the addition of antibacterial agents such as antibiotics can cause bacterial drug resistance. Graphene is found to have an antibacterial effect through mechanical damage and oxidative stress, etc., which avoids the problem of bacterial resistance. The porous structure has good porosity, can be well adhered to target cells, and has the effect of promoting osteoblast proliferation and differentiation.
At present, no report of preparing a nest-shaped ordered porous graphene coating on the surface of a titanium implant material is found in the prior art.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of a honeycomb-shaped ordered porous graphene coating.
The technical scheme is as follows:
a preparation method of a honeycomb-shaped ordered porous graphene coating comprises the following steps:
step 1, GO preparation: 46ml of 98% concentrated H2SO42g of expanded graphite 500nm and 1g of NaNO3Adding the mixture into a 250mL round-bottom flask, and stirring in an ice-water bath; then 6g KMnO were added in six portions over 1 hour4Adding into a round-bottom flask, and then continuing stirring for 2 hours; replacing ice water bath with oil bath, raising the temperature to 35-40 deg.c and maintaining the reaction for 1.5 hr; oxidized at this stageThe process is started slowly, and the viscosity of the system rises continuously; then, 100mL of deionized water is added into the system, the temperature of the system is controlled to be rapidly increased to 98 ℃, and the stirring is continued for 2.5 hours at the temperature; finally, H is slowly dropped into the system2O2Solution until no bubbles are generated;
step 2, ultrasonically cleaning the polished titanium sheet in deionized water, ethanol, acetone and deionized water for 10 minutes respectively, and drying the titanium sheet by nitrogen;
and 3, preparing the Ti surface porous GO coating by adopting a phase transfer combined Breath-Figure self-assembly method.
Further, the specific process of step 3 is: firstly, ultrasonically dispersing GO in deionized water to form stable dispersion liquid, centrifuging at high speed to obtain liquid with an upper layer mainly comprising single-layer GO, adjusting the pH to 9.0 by using 1M NaOH, then adding a chloroform solution containing a DODA cationic surfactant, forming a GO.DODA complex by electrostatic interaction between negative charges on the surface of GO and positive charges carried by DODA, and transferring GO from a water phase to a chloroform phase; dripping a chloroform solution of GO onto the surface of Ti, introducing wet air flow, quickly volatilizing chloroform to cause water vapor to condense on the surface of GO to form a water drop template, self-assembling an ordered porous GO structure, and reserving the porous structure after water drops are evaporated; and reducing the obtained porous GO layer by adopting ascorbic acid to obtain a porous graphene coating.
The invention has the beneficial effects that:
according to the invention, the honeycomb-shaped ordered porous graphene coating is prepared on the surface of the titanium material, and the prepared coating not only can provide antibacterial property, but also can regulate and control the function of osteoblasts and promote the rapid osseointegration of the bone-titanium material.
Drawings
FIG. 1 is a flow chart of graphene oxide reagent addition prepared by the Hummers method;
FIG. 2A flow chart of the preparation of a Ti surface porous GO coating by using a phase transfer combined Breath-Figure self-assembly method.
Detailed Description
The technical solutions of the present invention will be described in further detail with reference to the accompanying drawings and the detailed description.
Preparation and characterization of 1 GO
GO is prepared by adopting an improved Hummers method, a reagent adding flow is shown in figure 1, and the detailed process is as follows:
46ml of 98% concentrated H2SO42g of expanded graphite (500nm) and 1g of NaNO3Added to a 250mL round bottom flask and stirred in an ice water bath. Then 6g KMnO were added in six portions over 1 hour4Added to the round bottom flask and then stirred for an additional 2 hours. The ice-water bath was replaced by an oil bath, the temperature was raised to 35 ℃ to 40 ℃ and the reaction was maintained for 1.5 hours. The oxidation process at this stage begins slowly and the viscosity of the system rises continuously. Then, 100mL of deionized water was added to the system, the temperature of the system was rapidly raised to 98 ℃ with control, and stirring was continued at this temperature for 2.5 hours. Finally, H is slowly dropped into the system2O2Solution until no bubbles are generated.
Washing the prepared GO by adopting a centrifugal method, subpackaging the obtained reaction liquid into different centrifugal tubes, adding a certain amount of deionized water, centrifuging at 6000rpm for 2min, and removing supernatant, wherein the step is repeated for multiple times until the supernatant liquid is in a foggy state. At this point, a pH test is performed and if the pH is between 6 and 7, collection can be performed. For the precipitate, sonication was continued for 30min with an amount of deionized water, followed by centrifugation and collection in the same manner to maximize yield.
After drying the prepared GO, taking a certain amount of powder, and measuring the oxygen content and the oxidation degree of the powder by using an element analyzer; ultrasonically dispersing GO in water, spin-coating to a mica sheet, and observing the size and the thickness of the mica sheet by adopting AFM; SP of carbon atom in GO2Hybrid and SP3Hybridization was characterized by Raman spectroscopy.
Self-assembly of 2 Ti surface ordered porous graphene coating
And ultrasonically cleaning the polished titanium sheet in deionized water, ethanol, acetone and deionized water for 10 minutes respectively, and drying by nitrogen.
The Ti surface porous GO coating is prepared by adopting a phase transfer combined Breath-Figure self-assembly method, the process is shown in Figure 2, GO is ultrasonically dispersed in deionized water to form stable dispersion liquid, liquid with an upper layer mainly being monolayer GO is obtained through high-speed centrifugation, the pH value is adjusted to 9.0 by 1M NaOH, then chloroform solution containing DODA cationic surfactant is added, a GO.DODA complex is formed by the electrostatic interaction between negative charges on the surface of GO and positive charges carried by DODA, and GO can be transferred from a water phase to a chloroform phase. Drip the chloroform solution of GO to the Ti surface, let in moist air current simultaneously, chloroform volatilizees rapidly, leads to vapor to condense on the GO surface, forms the water droplet template, and the orderly porous GO structure of self-assembly waits the water droplet evaporation back, and porous structure remains. And reducing the obtained porous GO layer by adopting ascorbic acid to obtain a porous graphene coating.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are within the scope of the present invention.
Claims (1)
1. A preparation method of a honeycomb-shaped ordered porous graphene coating is characterized by comprising the following steps:
step 1, GO preparation: 46mL of 98% concentrated H2SO42g of expanded graphite 500nm and 1g of NaNO3Adding the mixture into a 250mL round-bottom flask, and stirring in an ice-water bath; then 6g KMnO were added in six portions over 1 hour4Adding into a round-bottom flask, and then continuing stirring for 2 hours; replacing ice water bath with oil bath, raising the temperature to 35-40 deg.c and maintaining the reaction for 1.5 hr; the oxidation process at this stage starts slowly, and the viscosity of the system rises continuously; then, 100mL of deionized water is added into the system, the temperature of the system is controlled to be rapidly increased to 98 ℃, and the stirring is continued for 2.5 hours at the temperature; finally, H is slowly dropped into the system2O2Solution until no bubbles are generated;
step 2, ultrasonically cleaning the polished titanium sheet in deionized water, ethanol, acetone and deionized water for 10 minutes respectively, and drying the titanium sheet by nitrogen;
step 3, preparing the Ti surface porous GO coating by adopting a phase transfer combined Breath-Figure self-assembly method, wherein the specific process is as follows: firstly, ultrasonically dispersing GO in deionized water to form stable dispersion liquid, centrifuging at high speed to obtain liquid with an upper layer mainly comprising single-layer GO, adjusting the pH value to 9.0 by using 1M NaOH, then adding a chloroform solution containing a DODA cationic surfactant, forming a GO-DODA complex by electrostatic interaction between negative charges on the surface of GO and positive charges on the surface of DODA, and transferring the GO from a water phase to a chloroform phase; dripping a chloroform solution of GO onto the surface of Ti, introducing wet air flow, quickly volatilizing chloroform to cause water vapor to condense on the surface of GO to form a water drop template, self-assembling an ordered porous GO structure, and reserving the porous structure after water drops are evaporated; and reducing the obtained porous GO layer by adopting ascorbic acid to obtain a porous graphene coating.
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基于聚乳酸和氧化石墨烯的功能化改性及生物医学应用研究;赵长虹;《中国博士学位论文全文数据库医药卫生科技辑》;20170215(第2期);第2.1、2.2.4、3.2.2、5.2.2、5.2.4小节 * |
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