CN106086842A - A kind of metal surface high biological compatibility coating and preparation method - Google Patents
A kind of metal surface high biological compatibility coating and preparation method Download PDFInfo
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- CN106086842A CN106086842A CN201610726884.8A CN201610726884A CN106086842A CN 106086842 A CN106086842 A CN 106086842A CN 201610726884 A CN201610726884 A CN 201610726884A CN 106086842 A CN106086842 A CN 106086842A
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- preparation
- hydroxyapatite
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- phosphonic acid
- ethylhexyl phosphonic
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/23—Condensed phosphates
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- Materials For Medical Uses (AREA)
Abstract
The invention provides the preparation method of a kind of metal surface high biological compatibility coating, after comprising the steps: that pending for metal sample is washed by (1), be soaked in two banks solution, the surface taking out dried metal sample prepares di 2 ethylhexyl phosphonic acid phosphating coat；(2) it is positioned over hydroxyapatite suspension after the metal sample washing after step (1) being processed to soak, is stirred simultaneously, take out and prepare hydroxyapatite coating layer after drying.The present invention is that the coating process mainly in combination with mode can realize the coating that hydroxyapatite quickly consolidates with chemical bonds, thus completes the preparation of biocompatible coatings.
Description
Technical field
The present invention relates to the preparation of coating for metal surfaces, particularly relate to a kind of metal surface high biological compatibility coating
Preparation method.
Background technology
At present, biological and medical experiment main carriers is glass drying oven, and operating theater instruments, embedded material and other medical treatment
The main material of equipment is medical alloy, and bio-compatibility is poor.Biological and medical science needs material a kind of to metal coating, and it is raw
Thing is compatible the most close with glass surface, thus the experiment the data obtained realizing carrying out on glass drying oven is mutual with metallic weapon
Logical.(hydroxyapatite, is abbreviated as HA or HAP to hydroxyapatite, and molecular formula is Ca10(OH)2(PO4)6) it is tooth and skeleton
Main (inorganic) composition, the most medically also serve as the optimal components of artificial bone.Hydroxylapatite biology compatibility is good, is
Can stimulate or induce bone growth and synosteotic natural ceramic material, bio-compatibility and life can be formed with osseous tissue
Thing activity is superior to tricalcium phosphate and other phosphorus calcium ceramic material.The use of hydroxyapatite, contributes to the adhesion of cell, propagation
And Function, on the basis of directly as the replacement such as bone, tooth or impairment renovation material, the most excellent bone tissue engineer
Carrier material, it is possible to as other medical science functional material or the carrier material of medicine.
Summary of the invention
Present invention aim to address subproblem present in existing metal substrate surface film technique, it is provided that Yi Zhongjin
Metal surface high biological compatibility coating and preparation method.
It is an object of the invention to be achieved through the following technical solutions:
The preparation method of a kind of metal surface high biological compatibility coating, comprises the steps:
(1), after pending for metal sample being washed, it is soaked in two banks solution, takes out the surface system of dried metal sample
Obtain chemically reactive layer and di 2 ethylhexyl phosphonic acid phosphating coat；
(2) it is positioned over hydroxyapatite suspension after the metal sample washing after step (1) being processed to soak, carries out simultaneously
Stirring, takes out dried prepared hydroxyapatite coating layer.
Preferably, in described step (1), soaking temperature is 20-30 DEG C, and the time is 1-5 minute；Two banks solution concentration is
0.6-5mol/l。
Preferably, described two banks solution is 1-hydroxy ethylidene-1,1-diphosphonic acid solution.
Preferably, the thickness of the di 2 ethylhexyl phosphonic acid phosphating coat in described step (1) is 10-1000 nanometer.
Preferably, the washing in described step (1) is deionized water supersound washing.
Preferably, the concentration of the hydroxyapatite suspension in described step (2) is 5-40g/l.
Preferably, the soaking temperature in described step (2) is 20-30 DEG C, and the time is 2-5 minute.
Preferably, dry in described step (1) and step (2) is and is positioned over 50-70 DEG C of dry 5-20 in dry case and divides
Clock or 20-30 DEG C of air drying 2-4 hour.
Preferably, the thickness of the hydroxyapatite coating layer in described step (2) is 10-1000 micron.
Another aspect of the invention is a kind of metal surface high biological compatibility coating, include metallic substrates, change successively
Learning conversion zone, di 2 ethylhexyl phosphonic acid phosphating coat and hydroxyapatite coating layer, the thickness of described di 2 ethylhexyl phosphonic acid phosphating coat is 10-1000 nanometer, hydroxyl
The thickness of base apatite coating is 10-1000 micron.
Beneficial effects of the present invention: the one biocompatible material efficient, easy that the present invention provides is in metal surface
Film build method, it is achieved itself and the chemical bonds of metallic substrates, improves the bio-compatible performance of metal surface.The present invention is applicable to respectively
Planting size, all kinds of metallic substrates, such as rustless steel, carbon steel, screw-thread steel, cold-rolled steel, hot-rolled steel, manganese steel, aluminum, aluminium alloy, titanium, titanium closes
Gold, cobalt alloy, the one of magnalium etc..Most metal medical appliances is all naked metallic weapon, and the present invention can be efficiently modified
Bio-compatible sex chromosome mosaicism, after the conversion chemosphere that di 2 ethylhexyl phosphonic acid phosphating coat is master is formed, can adsorb hydroxyl at metallic surface
Apatite powder film forming.This is that the coating process mainly in combination with mode can realize hydroxyapatite and quickly consolidates with chemical bonds
Coating, thus the preparation completing biocompatible coatings is different from the side of the complex and expensive such as physically or chemically vapour deposition
Method.
Accompanying drawing explanation
Fig. 1 is the Rotating fields schematic diagram of product of the present invention；
Fig. 2 is the fluorescence distribution of the AnnexinV-FITC of embodiment 1 product；
Fig. 3 is the fluorescence distribution of the AnnexinV-FITC of embodiment 2 product；
Fig. 4 is the fluorescence distribution of the AnnexinV-FITC of embodiment 3 product；
Fig. 5 is the fluorescence distribution of the AnnexinV-FITC with reference to negative staining cell；
Fig. 6 is the PI dye marker non-viable apoptotic cell fluorescence distribution of embodiment 1 product；
Fig. 7 is the PI dye marker non-viable apoptotic cell fluorescence distribution of embodiment 2 product；
Fig. 8 is the PI dye marker non-viable apoptotic cell fluorescence distribution of embodiment 3 product；
Fig. 9 is the PI dye marker non-viable apoptotic cell fluorescence distribution with reference to negative staining cell；
Figure 10 is the photoelectron spectrograph detection schematic diagram of embodiment 4 product.
Detailed description of the invention
In order to the present invention is better described, below in conjunction with the accompanying drawing in the embodiment of the present invention, in the embodiment of the present invention
Technical scheme is clearly and completely described.
A kind of metal surface high biological compatibility coating, including metallic substrates 12, metal surface 13, chemically reactive layer
14, di 2 ethylhexyl phosphonic acid phosphating coat 18 and hydroxyapatite coating layer 16, di 2 ethylhexyl phosphonic acid phosphating coat 18 thickness can be controlled in 10-1000 nanometer, hydroxyl
The thickness of base apatite coating 16 is 10-1000 micron.
Preparation method is as follows: foreign material or the dirts such as the metallic substrates 12 of the pending sample of metal and oxide on surface (such as rust)
Dye thing, is demarcated as fresh metal surface 13 in the middle of it；After pending for metal sample deionized water supersound washing, put into room temperature
In 5mol/l 1-hydroxy ethylidene-1,1-diphosphonic acid solution, soak 2 minutes, remove the foreign material such as oxide on surface (rust), and in metal surface
One layer of chemically reactive layer 14 based on diphosphate is formed on 13.The formation of this layer of salt refers to quote document, if desired may be used
Use deaerating plant.
The metal sample processed is taken out and is dried in atmosphere, chemically reactive layer 14 can be formed one layer of di 2 ethylhexyl phosphonic acid phosphatization
Film 18, thickness can be 500 nanometers, and unnecessary phosphating coat can be rinsed out by current.
After di 2 ethylhexyl phosphonic acid phosphating coat 18 is formed, constantly it is stirred the above-mentioned metal sample processed at 20 DEG C soaking
Placing 5 minutes in hydroxyapatite (HA) suspension of 20g/l, the hydroapatite particles being suspended in water will be at di 2 ethylhexyl phosphonic acid phosphorus
The surface changing film 18 forms hydroxyapatite coating layer 16, and thickness is 500 microns.
Embodiment 1:
(1) people's gastric mucosal cell strain (GES-1) is positioned on glass sample cultivation 60 hours, collects cell, use thin
Born of the same parents' apoptosis test kit dyes, and detects the fluorescence signal of AnnexinV-FITC and PI on BD-Accuri C6 flow cytometer.
AnnexinV-FITC labelling viable apoptotic cell, PI labelling non-viable apoptotic cell.
Embodiment 2:
(1) by 304 stainless steel carriers with after deionized water supersound washing, 20 DEG C are soaked in 5mol/l 1-hydroxy ethylidene-1,1-diphosphonic acid
In 2 minutes, be positioned in 70 DEG C of drying baker be dried 20 minutes；
(2), after being washed with deionized by (1) step gained stainless steel carrier, the hydroxyapatite being positioned over 20g/l hangs
In turbid liquid, constantly it is stirred 20 DEG C and soaks 5 minutes；
(3) (2) step gained stainless steel carrier is positioned over 60 DEG C of temperature in drying baker and is dried 10 minutes；
(4) (3) step gained sample is positioned in deionized water flushing 30 seconds；
(5) (4) step gained sample is positioned over 60 DEG C of temperature in drying baker and is dried 10 minutes；
(6) people's gastric mucosal cell strain (GES-1) is positioned on (5) sample cultivation 60 hours, collects cell, use cell
Apoptosis test kit dyes, and detects the fluorescence signal of AnnexinV-FITC and PI on BD-Accuri C6 flow cytometer.
AnnexinV-FITC labelling viable apoptotic cell, PI labelling non-viable apoptotic cell.
Embodiment 3:
(1) by 304 stainless steel carriers with after deionized water supersound washing, it is positioned in 70 DEG C of drying baker and is dried 20 minutes；
(2), after being washed with deionized by (1) step gained stainless steel carrier, the hydroxyapatite being positioned over 20g/l hangs
In turbid liquid, constantly it is stirred 20 DEG C and soaks 5 minutes；
(3) (2) step gained stainless steel carrier is positioned over 60 DEG C of temperature in drying baker and is dried 10 minutes；
(4) (3) step gained sample is positioned in deionized water flushing 30 seconds；
(5) (4) step gained sample is positioned over 60 degree of temperature in drying baker and is dried 10 minutes；
(6) people's gastric mucosal cell strain (GES-1) is positioned on (5) sample cultivation 60 hours, collects cell, use cell
Apoptosis test kit dyes, and detects the fluorescence signal of AnnexinV-FITC and PI on BD-Accuri C6 flow cytometer.
AnnexinV-FITC labelling viable apoptotic cell, PI labelling non-viable apoptotic cell.
Embodiment 4:
(1) by 304 stainless steel carriers with after deionized water supersound washing, 20 DEG C are soaked in 5mol/l 1-hydroxy ethylidene-1,1-diphosphonic acid
In (etidronic acid, HEDP) 2 minutes, it is positioned in 70 DEG C of drying baker and is dried 20 minutes；
(2), after being washed with deionized by (1) step gained stainless steel carrier, it is positioned over the hydroxyapatite of 20g/l
(HA), in suspension, constantly it is stirred 20 DEG C and soaks 5 minutes；
(3) (2) step gained stainless steel carrier is positioned over 60 DEG C of temperature in drying baker and is dried 10 minutes；
(4) (3) step gained sample is positioned in deionized water flushing 30 seconds；
(5) (4) step gained sample is positioned over 60 DEG C of temperature in drying baker and is dried 10 minutes；Photoelectron energy is put into after taking
Spectrometer (XPS) detects.
The fluorescence distribution of the AnnexinV-FITC of Fig. 2-4 display embodiment 1-3 product.Fig. 5 is with reference to negative staining cell
The fluorescence distribution of the AnnexinV-FITC of comparison, Annexin negative marker is less than 105.Embodiment 1, embodiment 2, embodiment
3 all there is positive distribution, and embodiment 2 viable apoptotic cell ratio is significantly lower than embodiment 1, embodiment 3, after prompting plated film
Bio-compatibility is substantially better than non-plated film steel plate.2 groups of viable apoptotic cells of embodiment are minimum, the bio-compatibility after prompting plated film
Excellent.
Fig. 6-8 display embodiment 1-3 product P I dye marker non-viable apoptotic cell fluorescence distribution: Fig. 9 is with reference to dyeing the moon
The PI dye marker non-viable apoptotic cell fluorescence distribution of sexual cell comparison, embodiment 1, embodiment 2 do not measure the obvious PI positive and divide
Cloth, and embodiment 3 has brighter existing positive distribution, the steel plate cytotoxicity after prompting plated film is reduced to close with glass.
Figure 10 is the photoelectron spectroscopy of embodiment 4, result show to employ di 2 ethylhexyl phosphonic acid as chemical binding layer after, metal watch
Face is coated with complete hydroxyapatite coating layer.
Test result illustrate, the embodiment of the present invention 2 employ di 2 ethylhexyl phosphonic acid as chemical binding layer after, can be with active adsorption
Hydroxylapatite ceramic powder body forms biocompatible coatings；Embodiments of the invention 3 are not used then to cannot be carried out coating.And
And, the biocompatibility of this coating is close with glass and is slightly better than glass.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection of claims
Scope is as the criterion.
Claims (10)
1. the preparation method of a metal surface high biological compatibility coating, it is characterised in that comprise the steps:
(1), after pending for metal sample being washed, it is soaked in two banks solution, takes out surface preparedization of dried metal sample
Learn conversion zone and di 2 ethylhexyl phosphonic acid phosphating coat；
(2) it is positioned over hydroxyapatite suspension after the metal sample washing after step (1) being processed to soak, stirs simultaneously
Mix, take out dried surface and prepare hydroxyapatite coating layer.
Preparation method the most according to claim 1, it is characterised in that in described step (1), soaking temperature is 20-30 DEG C,
Time is 1-5 minute；Two banks solution concentration is 0.6-5mol/l.
Preparation method the most according to claim 2, it is characterised in that described two banks solution is that 1-hydroxy ethylidene-1,1-diphosphonic acid is molten
Liquid.
Preparation method the most according to claim 1, it is characterised in that the thickness of the di 2 ethylhexyl phosphonic acid phosphating coat in described step (1)
Degree is 10-1000 nanometer.
Preparation method the most according to claim 1, it is characterised in that the washing in described step (1) is that deionized water surpasses
Sound washs.
Preparation method the most according to claim 1, it is characterised in that the hydroxyapatite suspension in described step (2)
Concentration be 5-40g/l.
Preparation method the most according to claim 1, it is characterised in that the soaking temperature in described step (2) is 20-30
DEG C, the time is 2-5 minute.
Preparation method the most according to claim 1, it is characterised in that dry in described step (1) and step (2) is
It is positioned in dry case 50-70 DEG C of dry 5-20 minute or 20-30 DEG C of air drying 2-4 hour.
Preparation method the most according to claim 1, it is characterised in that the hydroxyapatite coating layer in described step (2)
Thickness is 10-1000 micron.
10. the metal surface high biological compatibility coating prepared according to the arbitrary described method of claim 1-9, its feature exists
In, include metallic substrates, chemically reactive layer, di 2 ethylhexyl phosphonic acid phosphating coat and hydroxyapatite coating layer, described di 2 ethylhexyl phosphonic acid phosphating coat successively
Thickness be 10-1000 nanometer, the thickness of hydroxyapatite coating layer is 10-1000 micron.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106620850A (en) * | 2017-01-17 | 2017-05-10 | 焦敬 | Biocompatible coating on surface of orthopedic implant and preparation method |
| CN106835095A (en) * | 2017-01-17 | 2017-06-13 | 李乃义 | Tooth-implanting surface biological compatibility coating and preparation method |
| CN107267973A (en) * | 2017-05-09 | 2017-10-20 | 西南交通大学 | A kind of method for building metal organic framework composite coating in magnesium based metal |
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| CN1791437A (en) * | 2003-05-16 | 2006-06-21 | 布卢薄膜有限责任公司 | Medical implants comprising biocompatible coatings |
| US20120288705A1 (en) * | 2010-11-08 | 2012-11-15 | The Board Of Regents For Oklahoma State University | Hydroxyapatite coated metal surface and method for producing |
| CN106075608A (en) * | 2016-06-03 | 2016-11-09 | 泰安市御翔医疗科技有限公司 | A kind of fibrin ferment sustained release medicine equipment and preparation method |
| CN205954109U (en) * | 2016-08-25 | 2017-02-15 | 济南御麟化工科技有限公司 | High biocompatibility coating of metal surface |
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2016
- 2016-08-25 CN CN201610726884.8A patent/CN106086842A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002098307A1 (en) * | 2001-06-07 | 2002-12-12 | The Royal Alexandra Hospital For Children | A device for the delivery of a drug to a fractured bone |
| CN1791437A (en) * | 2003-05-16 | 2006-06-21 | 布卢薄膜有限责任公司 | Medical implants comprising biocompatible coatings |
| US20120288705A1 (en) * | 2010-11-08 | 2012-11-15 | The Board Of Regents For Oklahoma State University | Hydroxyapatite coated metal surface and method for producing |
| CN106075608A (en) * | 2016-06-03 | 2016-11-09 | 泰安市御翔医疗科技有限公司 | A kind of fibrin ferment sustained release medicine equipment and preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106620850A (en) * | 2017-01-17 | 2017-05-10 | 焦敬 | Biocompatible coating on surface of orthopedic implant and preparation method |
| CN106835095A (en) * | 2017-01-17 | 2017-06-13 | 李乃义 | Tooth-implanting surface biological compatibility coating and preparation method |
| CN107267973A (en) * | 2017-05-09 | 2017-10-20 | 西南交通大学 | A kind of method for building metal organic framework composite coating in magnesium based metal |
| CN107267973B (en) * | 2017-05-09 | 2019-07-19 | 西南交通大学 | A method of metal-organic framework composite coating is constructed in magnesium based metal |
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Application publication date: 20161109 |