CN105970191A - Method for preparing anti-coagulation zinc oxide film on copper surface - Google Patents
Method for preparing anti-coagulation zinc oxide film on copper surface Download PDFInfo
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- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- A61L33/00—Antithrombogenic treatment of surgical articles, e.g. sutures, catheters, prostheses, or of articles for the manipulation or conditioning of blood; Materials for such treatment
- A61L33/0005—Use of materials characterised by their function or physical properties
- A61L33/0011—Anticoagulant, e.g. heparin, platelet aggregation inhibitor, fibrinolytic agent, other than enzymes, attached to the substrate
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- A61L33/00—Antithrombogenic treatment of surgical articles, e.g. sutures, catheters, prostheses, or of articles for the manipulation or conditioning of blood; Materials for such treatment
- A61L33/18—Use of ingredients of undetermined constitution or reaction products thereof
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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- C23C18/1241—Metallic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/418—Agents promoting blood coagulation, blood-clotting agents, embolising agents
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Abstract
The invention discloses a method for preparing an anti-coagulation zinc oxide film on the surface of a copper sheet. By preparing the nano-zinc oxide film with super-hydrophobic performance on the surface of the copper sheet, the adhesion amount of blood platelets on the surface of the film can be effectively reduced, and the copper sheet is made to achieve good anti-coagulation performance. According to the method, the zinc oxide film is prepared through the technique combining electro-deposition with a hydrothermal method, the copper sheet is fixed to one end of an electrode and placed into a precursor solution for electro-deposition, a zinc oxide seed layer is prepared on the surface of the copper sheet, then a certain temperature and time are controlled through the hydrothermal method, sintering is conducted at a certain temperature, and the anti-coagulation performance of the copper sheet is tested. The method is low in production cost, the preparation method is simple, the requirement for reaction equipment is low, reaction conditions are mild, environmental pollution is avoided, and large-scale production can be achieved.
Description
Technical field
The present invention relates to a kind of method preparing anticoagulation zinc-oxide film on copper surface.
Background technology
Biomaterial is that a class can be used for the reparation of animal organ and tissue and replacement, the Clinics and Practices of disease, compatible with animal organism, have the material of property or function.Anticoagulant biomaterial is the important component part of biomaterial, be widely used in on human blood and the medical material that contacts of tissue, such as hemodialysis system, extracorporeal circulation system, Cardiac valve prosthesis, cardiac pacemaker, artificial blood vessel, intravascular stent, surgical cable and conduit etc..Based on coronary artery and the Atherosclerotic cardiovascular disease of peripheral cardiovascular disease, it it is one of mortality rate is the highest in the world disease.2010, only in the U.S., for the expense the most up to 448,500,000,000 dollars of cardiovascular disease.The market of anticoagulant material is the hugest, and increases with the speed of annual 10% 20%.Therefore the anticoagulant property studying zinc oxide makes great sense.
Summary of the invention
In order to study the anticoagulation function on zinc-oxide film surface, the invention provides a kind of method preparing anticoagulation zinc-oxide film on copper sheet surface.
The technical solution used in the present invention is: a kind of method preparing anticoagulation zinc-oxide film on copper sheet surface, it is characterized in that: by preparing the zinc nitrate solution of certain concentration, with constant voltage dc source, cleaned copper sheet of polishing is carried out electro-deposition, preparation Seed Layer, sample is put in reactor, pour the Zn (NO of equimolar ratio into3)2·6H2O and NH3 .H2The mixed solution of O, takes out after reaction a period of time under given conditions, calcines, then measure its surface static contact angle, chooses super-hydrophobic/super hydrophilic sample and puts in platelet solution centrifugal, makes platelet adhesion reaction on thin film, observe under scanning electron microscope.
The present invention to prepare feature process step as follows:
One, compound concentration is the Zn (NO of 0.01 mol/L to 0.05 mol/L3)2·6H2O solution, is fixed on one end of electrode by clean copper sheet, carries out electro-deposition with the DC source of 2 V in the electrodeposit liquid of 50 DEG C to 90 DEG C, and sedimentation time is 10 min；
Two, configuration concentration is the Zn (NO of 0.02 mol/L to 0.08 mol/L3)2·6H2O solution, instills the NH of equimolar ratio in solution3 .H2O, stirs；
Three, the copper sheet having Seed Layer is put in reactor, then solution step 2 configured is poured in reactor, then the reactor of good seal is inserted in calorstat.2 h to 4 h is reacted in the atmospheric atmosphere of 70 DEG C to 90 DEG C；
Four, taking-up reactor is after it is down to room temperature, is taken out by sample, puts into Muffle furnace after being washed with deionized.Temperature is set to 200 DEG C, and temperature retention time is 2 h；
Five, take out sample after it cools down, measure the static contact angle of surface of nanometer zinc oxide with contact angle measurement；
Six, take the fresh blood of human body of 5 mL, shake up, centrifugal (3650 r/min) 10 min.Draw whole supernatant to another centrifuge tube, recentrifuge (3000 r/min) 10 min.The 3/4 of abandoning supernatant, remaining liq is high concentration thrombocyte plasma；
Seven, the phosphate buffer taking 20 uL high concentration thrombocyte plasma PH=7.4 dilutes 20 times, obtains platelet solution；
Eight, sample being immersed in platelet solution, be then centrifuged 1 min with 3500 r/min rotating speeds, rinse with phosphate buffer, 2.0% glutaraldehyde fixes 1 h, then by ethanol series dehydration, acetone dealcoholysis；
Nine, observe under scanning electron microscope platelet PLA2, build up, the situation such as deformation, to each sample, randomly select 3 equally distributed regions and take pictures.Observe and hematoblastic stick quantity and hematoblastic form.
Further, described step one prepares Seed Layer by electro-deposition.
Further, described step 2 adds NH3 .H2The amount of O is that solution is changed into clarification by muddiness just.
Further, reactor cooling in described step 4, with a large amount of cold water fast coolings, at a temperature of taking-up sample is placed on 200 DEG C, carries out in atmosphere, do not contain other protective gas.
Further, described step 5 is prepared there is super hydrophilic or super-hydrophobic sample.
Further, centrifugal blood is obtained by described step 6 high concentration thrombocyte plasma.
Further, in described step 8, platelet adhesion reaction is on copper sheet, protects its microscopic pattern.
Further, described step 9 is observed hematoblastic form, adds up hematoblastic quantity.
The invention have the advantage that the preparation of (1) Seed Layer so that the adhesion between zinc oxide and copper sheet is fine, overcome the zinc oxide generally existed and hold a flaky difficult problem；(2) preparing zinc oxide by hydro-thermal method on copper sheet surface, zinc oxide is evenly distributed, Stability Analysis of Structures；(3) zinc oxide is a kind of wide bandgap semiconductor materials, and has good biocompatibility, and its hydrophobic surface makes device be difficult to pollute, and sterilization easy to clean, is the most promising anticoagulant material.(4) zinc nitrate of present invention use, ammonia etc. are all conventional raw materials, and production cost is low, requires low to consersion unit, and reaction condition is gentle, and preparation method is simple, non-environmental-pollution.
Accompanying drawing explanation
Fig. 1 is the field emission scanning electron microscope figure of zinc-oxide film of the present invention；
Fig. 2 is the platelet adhesion reaction of the present invention SEM figure on zinc-oxide film；
Fig. 3 is the schematic diagram of platelet adhesion reaction quantity of the present invention and contact angle relation.
Detailed description of the invention
Provide embodiments of the invention and the present invention be illustrated by embodiment that combination is given, but the present invention is not constituted any limitation by given embodiment:
Detailed description of the invention one: compound concentration is the Zn (NO of 0.01 mol/L3)2·6H2O solution, is fixed on one end of electrode by clean copper sheet, carries out electro-deposition with the DC source of 2 V in the electrodeposit liquid of 50 DEG C, and sedimentation time is 10 min；Configuration concentration is the Zn (NO of 0.05 mol/L3)2·6H2O solution, instills the NH of equimolar ratio in solution3 .H2O, stirs；The copper sheet having Seed Layer is put in reactor, then solution step 2 configured is poured in reactor, then the reactor of good seal is inserted in calorstat.4 h are reacted in the atmospheric atmosphere of 90 DEG C；Sample, after it is down to room temperature, is taken out, puts into Muffle furnace after being washed with deionized by taking-up reactor.Temperature is set to 200 DEG C, and temperature retention time is 2 h；
Taking out sample and measure the static contact angle of surface of nanometer zinc oxide after it cools down with contact angle measurement, the static contact angle recording this sample surfaces is 167.7 °, and roll angle is 6.7 °；Take the fresh blood of human body of 5 mL, shake up, centrifugal (3650 r/min) 10 min.Draw whole supernatant to another centrifuge tube, recentrifuge (3000 r/min) 10 min.The 3/4 of abandoning supernatant, remaining liq is high concentration thrombocyte plasma；The phosphate buffer taking 20 uL high concentration thrombocyte plasma PH=7.4 dilutes 20 times, obtains platelet solution；Sample being immersed in platelet solution, is then centrifuged 1 min with 3500 r/min rotating speeds, rinse with phosphate buffer, 2.0% glutaraldehyde fixes 1 h, then by ethanol series dehydration, acetone dealcoholysis.
Observe under scanning electron microscope platelet PLA2, build up, the situation such as deformation, to each sample, randomly select 3 equally distributed regions and take pictures.Observing and hematoblastic stick quantity and hematoblastic form, estimating hematoblastic quantity of sticking by SEM picture is 0.74 × 104Individual/cm2. hematoblastic form does not changes yet, and illustrates that platelet is not activated, and this material has good anticoagulant functions.
Detailed description of the invention two: compound concentration is the Zn (NO of 0.01 mol/L3)2·6H2O solution, is fixed on one end of electrode by clean copper sheet, carries out electro-deposition with the DC source of 2 V in the electrodeposit liquid of 90 DEG C, and sedimentation time is 10 min；Configuration concentration is the Zn (NO of 0.05 mol/L3)2·6H2O solution, instills the NH of equimolar ratio in solution3 .H2O, stirs；The copper sheet having Seed Layer is put in reactor, then solution step 2 configured is poured in reactor, then the reactor of good seal is inserted in calorstat.4 h are reacted in the atmospheric atmosphere of 90 DEG C；Sample, after it is down to room temperature, is taken out, puts into Muffle furnace after being washed with deionized by taking-up reactor.Temperature is set to 200 DEG C, and temperature retention time is 2 h；
Taking out sample and measure the static contact angle of surface of nanometer zinc oxide after it cools down with contact angle measurement, the static contact angle recording this sample surfaces is 3.7 °；Take the fresh blood of human body of 5 mL, shake up, centrifugal (3650 r/min) 10 min.Draw whole supernatant to another centrifuge tube, recentrifuge (3000 r/min) 10 min.The 3/4 of abandoning supernatant, remaining liq is high concentration thrombocyte plasma；The phosphate buffer taking 20 uL high concentration thrombocyte plasma PH=7.4 dilutes 20 times, obtains platelet solution；Sample being immersed in platelet solution, is then centrifuged 1 min with 3500 r/min rotating speeds, rinse with phosphate buffer, 2.0% glutaraldehyde fixes 1h, then by ethanol series dehydration, acetone dealcoholysis.
Observe under scanning electron microscope platelet PLA2, build up, the situation such as deformation, to each sample, randomly select 3 equally distributed regions and take pictures.Observing and hematoblastic stick quantity and hematoblastic form, estimating hematoblastic quantity of sticking by SEM picture is 1.36 × 104Individual/cm2. hematoblastic form does not changes yet, and illustrates that platelet is not activated, and the anticoagulant functions of this material is general.
Detailed description of the invention three: compound concentration is the Zn (NO of 0.05 mol/L3)2·6H2O solution, is fixed on one end of electrode by clean copper sheet, carries out electro-deposition with the DC source of 2 V in the electrodeposit liquid of 70 DEG C, and sedimentation time is 10 min；Configuration concentration is the Zn (NO of 0.05 mol/L3)2·6H2O solution, instills the NH of equimolar ratio in solution3 .H2O, stirs；The copper sheet having Seed Layer is put in reactor, then solution step 2 configured is poured in reactor, then the reactor of good seal is inserted in calorstat.4 h are reacted in the atmospheric atmosphere of 90 DEG C；Sample, after it is down to room temperature, is taken out, puts into Muffle furnace after being washed with deionized by taking-up reactor.Temperature is set to 200 DEG C, and temperature retention time is 2 h；
Taking out sample and measure the static contact angle of surface of nanometer zinc oxide after it cools down with contact angle measurement, the static contact angle recording this sample surfaces is 4.8 °；Take the fresh blood of human body of 5 mL, shake up, centrifugal (3650 r/min) 10 min.Draw whole supernatant to another centrifuge tube, recentrifuge (3000 r/min) 10 min.The 3/4 of abandoning supernatant, remaining liq is high concentration thrombocyte plasma；The phosphate buffer taking 20 uL high concentration thrombocyte plasma PH=7.4 dilutes 20 times, obtains platelet solution；Sample being immersed in platelet solution, is then centrifuged 1 min with 3500 r/min rotating speeds, rinse with phosphate buffer, 2.0% glutaraldehyde fixes 1 h, then by ethanol series dehydration, acetone dealcoholysis.
Observe under scanning electron microscope platelet PLA2, build up, the situation such as deformation, to each sample, randomly select 3 equally distributed regions and take pictures.Observing and hematoblastic stick quantity and hematoblastic form, estimating hematoblastic quantity of sticking by SEM picture is 1.48 × 104Individual/cm2. hematoblastic form does not changes yet, and illustrates that platelet is not activated, and the anticoagulant functions of this material is general.
Detailed description of the invention four: compound concentration is the Zn (NO of 0.01 mol/L3)2·6H2O solution, is fixed on one end of electrode by clean copper sheet, carries out electro-deposition with the DC source of 2 V in the electrodeposit liquid of 70 DEG C, and sedimentation time is 10 min；Configuration concentration is the Zn (NO of 0.05 mol/L3)2·6H2O solution, instills the NH of equimolar ratio in solution3 .H2O, stirs；The copper sheet having Seed Layer is put in reactor, then solution step 2 configured is poured in reactor, then the reactor of good seal is inserted in calorstat.4 h are reacted in the atmospheric atmosphere of 70 DEG C；Sample, after it is down to room temperature, is taken out, puts into Muffle furnace after being washed with deionized by taking-up reactor.Temperature is set to 200 DEG C, and temperature retention time is 2 h；
Taking out sample and measure the static contact angle of surface of nanometer zinc oxide after it cools down with contact angle measurement, the static contact angle recording this sample surfaces is 25.4 °；Take the fresh blood of human body of 5 mL, shake up, centrifugal (3650 r/min) 10 min.Draw whole supernatant to another centrifuge tube, recentrifuge (3000 r/min) 10 min.The 3/4 of abandoning supernatant, remaining liq is high concentration thrombocyte plasma；The phosphate buffer taking 20 uL high concentration thrombocyte plasma PH=7.4 dilutes 20 times, obtains platelet solution；Sample being immersed in platelet solution, is then centrifuged 1 min with 3500 r/min rotating speeds, rinse with phosphate buffer, 2.0% glutaraldehyde fixes 1 h, then by ethanol series dehydration, acetone dealcoholysis.
Observe under scanning electron microscope platelet PLA2, build up, the situation such as deformation, to each sample, randomly select 3 equally distributed regions and take pictures.Observing and hematoblastic stick quantity and hematoblastic form, estimating hematoblastic quantity of sticking by SEM picture is 2.03 × 104Individual/cm2. hematoblastic form does not changes yet, and illustrates that platelet is not activated, and the anticoagulant functions of this material is general.
Claims (7)
1. the method preparing anticoagulation zinc-oxide film on copper surface, it is characterized in that: prepared the zinc oxide seed layer with specific array density and thickness by electrodeposition process, then the super-hydrophobic zinc-oxide film with specific microscopic appearance is prepared by hydro-thermal method, prove that super-hydrophobic zinc-oxide film has anticoagulant property, sequentially include the following steps:
Compound concentration is the Zn (NO of 0.01 mol/L to 0.05 mol/L3)2·6H2O solution, is fixed on one end of electrode by clean copper sheet, carries out electro-deposition with the DC source of 2 V in the electrodeposit liquid of 50 DEG C to 90 DEG C, and sedimentation time is 10 min；
Configuration concentration is the Zn (NO of 0.02 mol/L to 0.08 mol/L3)2·6H2O solution, instills the NH of equimolar ratio in solution3 .H2O, stirs；
The copper sheet having Seed Layer is put in reactor, then solution step 2 configured is poured in reactor, then the reactor of good seal is inserted in calorstat；
2 h to 4 h is reacted under conditions of 70 DEG C to 90 DEG C；
Sample, after it is down to room temperature, is taken out, puts into Muffle furnace after being washed with deionized by taking-up reactor；
Temperature is set to 200 DEG C, and temperature retention time is 2 h；
Take out sample after it cools down, measure the static contact angle of surface of nanometer zinc oxide with contact angle measurement；
Take the fresh blood of human body of 5 mL, shake up, centrifugal (3650 r/min) 10 min；
Draw whole supernatant to another centrifuge tube, recentrifuge (3000
R/min) 10 min；
The 3/4 of abandoning supernatant, remaining liq is high concentration thrombocyte plasma；
The phosphate buffer taking 20 uL high concentration thrombocyte plasma PH=7.4 dilutes 20 times, obtains platelet solution；
Sample being immersed in platelet solution, is then centrifuged 1 min with 3500 r/min rotating speeds, rinse with phosphate buffer, 2.0% glutaraldehyde fixes 1 h, then by ethanol series dehydration, acetone dealcoholysis；
Observe under scanning electron microscope platelet PLA2, build up, the situation such as deformation, to each sample, randomly selecting 3 equally distributed regions takes pictures, and finds that hematoblastic quantity of sticking is little, shows obvious anticoagulant property.
A kind of method preparing anticoagulation zinc-oxide film on copper surface the most according to claim 1, it is characterised in that: described step one prepares Seed Layer by electro-deposition.
A kind of method preparing anticoagulation zinc-oxide film on copper surface the most according to claim 1, it is characterised in that: described step 2 adds NH3 .H2The amount of O is that solution is changed into clarification by muddiness just.
A kind of method preparing anticoagulation zinc-oxide film on copper surface the most according to claim 1; it is characterized in that: reactor cooling in described step 4, with a large amount of cold water fast coolings, at a temperature of taking-up sample is placed on 200 DEG C; carry out in atmosphere, do not contain other protective gas.
A kind of method preparing anticoagulation zinc-oxide film on copper surface the most according to claim 1, it is characterised in that: described step 5 is prepared there is super-hydrophobic zinc-oxide film.
A kind of method preparing anticoagulation zinc-oxide film on copper surface the most according to claim 1, it is characterised in that: by centrifugal blood in described step 6, it is thus achieved that high concentration thrombocyte plasma.
A kind of method preparing anticoagulation zinc-oxide film on copper surface the most according to claim 1, it is characterised in that: in described step 8, platelet adhesion reaction quantity on copper sheet is little.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111155089A (en) * | 2020-01-20 | 2020-05-15 | 南昌航空大学 | Preparation method of durable anti-ice super-hydrophobic stainless steel coating |
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| CN104357827A (en) * | 2014-11-03 | 2015-02-18 | 中国石油大学(华东) | Preparation method for super-hydrophobic corrosion-resistant copper-based surface |
| CN104674197A (en) * | 2015-01-31 | 2015-06-03 | 南昌航空大学 | Method for preparing ice-coating resistant zinc oxide coating on copper surface |
| CN105463564A (en) * | 2015-11-30 | 2016-04-06 | 东南大学 | ZnO nanorod and ZnO cluster composite structure and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111155089A (en) * | 2020-01-20 | 2020-05-15 | 南昌航空大学 | Preparation method of durable anti-ice super-hydrophobic stainless steel coating |
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