CN106283160A - A kind of preparation method of medical metal-based biological coating - Google Patents
A kind of preparation method of medical metal-based biological coating Download PDFInfo
- Publication number
- CN106283160A CN106283160A CN201610636146.4A CN201610636146A CN106283160A CN 106283160 A CN106283160 A CN 106283160A CN 201610636146 A CN201610636146 A CN 201610636146A CN 106283160 A CN106283160 A CN 106283160A
- Authority
- CN
- China
- Prior art keywords
- magnesium alloy
- plate
- coating
- standby
- medical metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- 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
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
-
- 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
- A61L27/32—Phosphorus-containing materials, e.g. apatite
-
- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
-
- 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
-
- 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
Abstract
The invention discloses the preparation method of a kind of medical metal-based biological coating, belong to metal coating layer material synthesis field.First the present invention cleans Mg alloy surface oil removing with acetone, after brushing Mel, immerse sea water and second pond activated sludge, invade Mg alloy surface growth corrosion through solar exposure catalysis sea water and microorganism in mud and algae, after drying sintering, make Mg alloy surface be formed with the component rich in hydroxyl of beneficially hydroxylapatite crystal, in electrophoretic deposition process, make matrix form chemical bonding with being coated with interlayer, be greatly improved interface bond strength, the most sintered obtain medical metal-based biological coating.Gained biological coating thickness is uniform, strong with basal body binding force, is difficult to loosen peeling during use, and the life-span is greatly improved.
Description
Technical field
The invention discloses the preparation method of a kind of medical metal-based biological coating, belong to metal coating layer material synthesis neck
Territory.
Background technology
Hydroxyapatite (is called for short HA), identical with the inorganic structural in skeleton, nontoxic, without ectosome after implantation human body
Reaction, has good biological activity and biocompatibility, is preferable skeleton substitution material.Research shows, porous HA
After implanting organism, the hard and soft tissue at interface can be made all to grow in space, form fibrous tissue and newly-generated osseous tissue cross knot
Conjunction state, this interface energy keeps normal metabolism relation, and the interfacial structure of bone-material has physiological and combines.But due to many
Hole HA belongs to fragile material, and intensity is low, poor toughness, and this just greatly limit its use as body implant.
Therefore effective ways are used to be coated with the metal-based compound obtained coated with biological activity HA coating in metal surface biological
Material, its surface activity having both the intensity of metal material, toughness and HA and biocompatibility.This material implants organism i.e.
Material-bone interface can be made to reach physiology combine, can effectively suppress again metal ion release in organism, be a kind of preferable
Novel biomaterial.
At present, the preparation method of coating for metal surfaces is a lot, mainly has metallikon, vapour deposition for its preparation technology
Method, roasting method, thermo chemical reaction, laser method and diffusion method etc..
Metallikon is to use ignition energy or electric energy that depositing materials (powder or granule) is melted or is atomized, cause molten state or
Semi-vitreous particle flux, and high velocity jet on ground and the method being piled into coating.Wherein plasma spray plating method is in recent years
Carry out development and application a kind of method faster.Use plasma spraying method can prepare the HA coating material of thickness G T.GT.GT 30 μm, be coated with
Layer and the bond strength > 60MPa of metallic substrates.But along with deeply finding with clinical practice of research, plasma spraying HA coating
Material remains in some problems, mainly: (1) cause due to linear spraying coating process the uneven of rough base face coat and
Cannot be carried out the face coat of complex shaped substrate;(2) the most clinical commonly used plasma spraying HA coating material is in system
Treatment temperature during Bei is the highest, sometimes even up to 10000K, makes coating produce interfacial stress in cooling procedure and residual
Stay in coating material, even make coating crack or after organism implanted by coating material, owing to long service is in body fluid
Environment make coating loosen or peel off.Simultaneously as the effect of high temperature easily makes HA decompose, in the coating produce impurity and
Amorphous HA and affect the biological property of coating.
It is HA fine powder to be made together with binding agent slurry be coated on base material that roasting method prepares the technique of HA coating, is dried
After, at a temperature of higher than 1000 DEG C, roasting forms, and its surface becomes ceramic coating after high temperature sintering.This coating has system
Standby technique is simple, and anchoring strength of coating is high, consistency advantages of higher.But it still uses high-temperature process, inevitably produces
The decomposition of HA and bioactive reduction.
The preparation method of biological coating material is more, but the coating material being applied to clinic up to now be also only limitted to etc. from
Sub-coating material, the limited main cause of the clinical practice of coating material is the interface cohesion problem of coating and matrix, except wait from
Outside sub-coating, the interface bond strength of the HA coating material prepared with additive method is below 20MPa.And plasma spraying HA is coated with
Although the interface bond strength of layer material may be up to 60MPa, but owing to there is aforesaid drawback, and make its clinically wide
General application have received restriction greatly.
Summary of the invention
Present invention mainly solves technical problem is that: occur in preparation process for conventional medical Metal Substrate biological coating
, the coating using plasma spraying to obtain is uneven, and treatment temperature is high, the most easily occurs that coating loosens and peels off,
The problem that the additive method gained coating interface bond strengths such as roasting are low, it is provided that the preparation of a kind of medical metal-based biological coating
Method.First the present invention cleans Mg alloy surface oil removing with acetone, after brushing Mel, immerses sea water and second pond activated sludge,
Invade Mg alloy surface growth corrosion through solar exposure catalysis sea water and microorganism in mud and algae, after drying sintering, make
Mg alloy surface is formed with the component rich in hydroxyl of beneficially hydroxylapatite crystal, in electrophoretic deposition process, make matrix with
It is coated with interlayer and forms chemical bonding, be greatly improved interface bond strength, the most sintered obtain medical metal-based biological coating.Gained
Biological coating thickness is uniform, strong with basal body binding force, is difficult to loosen peeling during use, and the life-span is greatly improved.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) intercept a size of 20mm × 16mm × 1mm and roll plate AZ31 magnesium alloy, be polishing to abrasive paper for metallograph that surface is uniform and smooth is
Only, clean magnesium alloy with acetone and roll plate surface 3~5 times, then be 75% alcohol washes 2~4 times by mass concentration, treat that surface is natural
After Feng Ganing, with hairbrush through artificial coating 10~12g Mel, then magnesium alloy plate rolled plate proceed in 75~80 DEG C of vacuum drying ovens,
Dried 2~4h, obtains pretreatment magnesium alloy and rolls plate, standby;
(2) in batch mixer, it is sequentially added into 2~4L sea water and 100~150g second pond activated sludge, starts and stir it, with 600
~800r/min rotating speed stirring mixing 20~30min, discharging, gained material is proceeded in closed glass container, then glass is held
Device is placed under sunlight, is exposed to the sun 3~5h;
(3) wait end of being exposed to the sun, step (1) standby pretreatment magnesium alloy is rolled plate and puts in above-mentioned glass container, be placed in sunlight
Under, airtight process 3~5 weeks of being exposed to the sun, take out, be washed with deionized 3~5 times, remove magnesium alloy and roll plate remained on surface mud, then
Magnesium alloy is rolled plate and proceeds in 80~85 DEG C of vacuum drying ovens, dried 3~5h;
(4) magnesium alloy after above-mentioned dry end is rolled plate and puts into Muffle furnace, be passed through nitrogen with 3~5mL/min speed, until row
Go out all air, be progressively warming up to 400~440 DEG C with 4~6 DEG C/min speed subsequently, heat preservation sintering under nitrogen guard mode
20~30min, stop heating, cool to room temperature with the furnace, obtain surface modification magnesium alloy and roll plate, standby;
(5) in beaker, being sequentially added into 20~30g600 mesh hydroxyapatite powders, 200~220mL mass concentrations are 75% second
Alcoholic solution, dropping mass concentration is 8~12% ammonia, regulates pH to 8.8~9.0, then is proceeded to by beaker in sonic oscillation instrument, with
10~12kHz power ultrasonic vibrations 5~8min, obtain unit for uniform suspension;
(6) rolling plate as negative electrode with step (4) standby surface modification magnesium alloy, carbon-point is anode, immerses and fills on 180~200mL
State in the electrolyzer of gained unit for uniform suspension, set electric field intensity as 5.2~5.8V/cm, electrophoretic deposition 40~60min, treat electricity
After swimming deposition terminates, cathode material is placed in 105~110 DEG C of baking ovens and is dried to constant weight, proceeded to Muffle furnace subsequently, at nitrogen
Under gas shielded state, it is heated to 720~780 DEG C, sintering processes 1~2h, cool to room temperature with the furnace, obtain medical metal-based
Biological coating.
The physical property of gained coating material of the present invention: gained of the present invention medical metal-based biological coating surface-brightening, nothing
Being mingled with, thickness is uniform, is 30~50 μm, and interface bond strength is 68~72MPa.
The invention has the beneficial effects as follows:
(1) present invention uses microbial pretreatment magnesium alloy materials, and surface treatment process is gentle and uniform, substantially increases alloy
Bond strength between material and coating, makes product be greatly improved service life, decreases raw-material consumption;
(2) processing procedure of the present invention is simple, need not put into large-scale jumbo, and production cost is low, environmental protection, can promote and make
With.
Detailed description of the invention
Intercept a size of 20mm × 16mm × 1mm and roll plate AZ31 magnesium alloy, be polishing to surface with abrasive paper for metallograph uniform and smooth
Till, clean magnesium alloy with acetone and roll plate surface 3~5 times, then be 75% alcohol washes 2~4 times by mass concentration, treat surface from
After so air-drying, with hairbrush through artificial coating 10~12g Mel, then magnesium alloy plate is rolled plate proceed to 75~80 DEG C of vacuum drying ovens
In, dried 2~4h, obtain pretreatment magnesium alloy and roll plate, standby;In batch mixer, be sequentially added into 2~4L sea water and 100~
150g second pond activated sludge, starts and stirs it, and with 600~800r/min rotating speeds stirring mixing 20~30min, discharging, by institute
Material proceeds in closed glass container, then glass container is placed under sunlight, is exposed to the sun 3~5h;Wait end of being exposed to the sun, by standby
Pretreatment magnesium alloy rolls plate and puts in above-mentioned glass container, is placed under sunlight, airtight process 3~5 weeks of being exposed to the sun, and takes out, spends
Ionized water washs 3~5 times, removes magnesium alloy and rolls plate remained on surface mud, then magnesium alloy rolls plate proceeds to 80~85 DEG C of vacuum and do
In dry case, dried 3~5h;Magnesium alloy after above-mentioned dry end is rolled plate and puts into Muffle furnace, with 3~5mL/min speed
Being passed through nitrogen, until discharging all air, being progressively warming up to 400~440 DEG C with 4~6 DEG C/min speed subsequently, protect at nitrogen
Heat preservation sintering 20~30min under state, stop heating, cool to room temperature with the furnace, obtain surface modification magnesium alloy and roll plate, standby;?
In beaker, being sequentially added into 20~30g600 mesh hydroxyapatite powders, 200~220mL mass concentrations are 75% ethanol solution, drip
Adding mass concentration is 8~12% ammonia, regulates pH to 8.8~9.0, then is proceeded to by beaker in sonic oscillation instrument, with 10~12kHz
Power ultrasonic vibration 5~8min, obtains unit for uniform suspension;Rolling plate as negative electrode with standby surface modification magnesium alloy, carbon-point is anode, leaching
Enter in the electrolyzer filling 180~200mL above-mentioned gained unit for uniform suspension, set electric field intensity as 5.2~5.8V/cm, electrophoresis
Deposition 40~60min, after electrophoretic deposition terminates, is placed in cathode material in 105~110 DEG C of baking ovens and is dried to constant weight, subsequently
Proceeded to Muffle furnace, under nitrogen guard mode, be heated to 720~780 DEG C, sintering processes 1~2h, cool to the furnace
Room temperature, obtains medical metal-based biological coating.
Example 1
Intercept a size of 20mm × 16mm × 1mm and roll plate AZ31 magnesium alloy, with abrasive paper for metallograph be polishing to surface uniform and smooth till,
Clean magnesium alloy with acetone and roll plate surface 3 times, then be 75% alcohol washes 2 times by mass concentration, after the natural air drying of surface, use
Hairbrush is through artificial coating 10g Mel, then magnesium alloy plate rolls plate proceeds in 75 DEG C of vacuum drying ovens, and dried 2h obtains pre-place
Reason magnesium alloy rolls plate, standby;In batch mixer, it is sequentially added into 2L sea water and 100g second pond activated sludge, starts and stir it, with
600r/min rotating speed stirring mixing 20min, discharging, gained material is proceeded in closed glass container, then glass container is placed in
Under sunlight, be exposed to the sun 3h;Wait end of being exposed to the sun, standby pretreatment magnesium alloy is rolled plate and puts in above-mentioned glass container, be placed in the sun
Under light, airtight process 3 weeks of being exposed to the sun, take out, be washed with deionized 3 times, remove magnesium alloy and roll plate remained on surface mud, then by magnesium
Alloy rolls plate and proceeds in 80 DEG C of vacuum drying ovens, dried 3h;Magnesium alloy after above-mentioned dry end is rolled plate and puts into Muffle
Stove, is passed through nitrogen with 3mL/min speed, until discharging all air, is progressively warming up to 400 DEG C with 4 DEG C/min speed subsequently,
Heat preservation sintering 20min under nitrogen guard mode, stops heating, cools to room temperature with the furnace, obtain surface modification magnesium alloy and roll plate, standby
With;In beaker, being sequentially added into 20g600 mesh hydroxyapatite powder, 200mL mass concentration is 75% ethanol solution, drips matter
Amount concentration is 8% ammonia, regulates pH to 8.8, then is proceeded to by beaker in sonic oscillation instrument, with 10kHz power ultrasonic vibration 5min,
Obtain unit for uniform suspension;Rolling plate as negative electrode with standby surface modification magnesium alloy, carbon-point is anode, immerses and fills the above-mentioned gained of 180mL
In the electrolyzer of unit for uniform suspension, set electric field intensity as 5.2V/cm, electrophoretic deposition 40min, after electrophoretic deposition terminates, will
Cathode material is placed in 105 DEG C of baking ovens and is dried to constant weight, is proceeded to Muffle furnace subsequently, and under nitrogen guard mode, heating rises
Warm to 720 DEG C, sintering processes 1h, cool to room temperature with the furnace, obtain medical metal-based biological coating.
Gained of the present invention medical metal-based biological coating surface-brightening, without being mingled with, thickness is uniform, is 30 μm, interface cohesion
Intensity is 68MPa.
Example 2
Intercept a size of 20mm × 16mm × 1mm and roll plate AZ31 magnesium alloy, with abrasive paper for metallograph be polishing to surface uniform and smooth till,
Clean magnesium alloy with acetone and roll plate surface 4 times, then be 75% alcohol washes 3 times by mass concentration, after the natural air drying of surface, use
Hairbrush is through artificial coating 11g Mel, then magnesium alloy plate rolls plate proceeds in 78 DEG C of vacuum drying ovens, and dried 3h obtains pre-place
Reason magnesium alloy rolls plate, standby;In batch mixer, it is sequentially added into 3L sea water and 120g second pond activated sludge, starts and stir it, with
700r/min rotating speed stirring mixing 25min, discharging, gained material is proceeded in closed glass container, then glass container is placed in
Under sunlight, be exposed to the sun 4h;Wait end of being exposed to the sun, standby pretreatment magnesium alloy is rolled plate and puts in above-mentioned glass container, be placed in the sun
Under light, airtight process 4 weeks of being exposed to the sun, take out, be washed with deionized 4 times, remove magnesium alloy and roll plate remained on surface mud, then by magnesium
Alloy rolls plate and proceeds in 82 DEG C of vacuum drying ovens, dried 4h;Magnesium alloy after above-mentioned dry end is rolled plate and puts into Muffle
Stove, is passed through nitrogen with 4mL/min speed, until discharging all air, is progressively warming up to 420 DEG C with 5 DEG C/min speed subsequently,
Heat preservation sintering 25min under nitrogen guard mode, stops heating, cools to room temperature with the furnace, obtain surface modification magnesium alloy and roll plate, standby
With;In beaker, being sequentially added into 25g600 mesh hydroxyapatite powder, 210mL mass concentration is 75% ethanol solution, drips matter
Amount concentration is 10% ammonia, regulates pH to 8.9, then is proceeded to by beaker in sonic oscillation instrument, with 11kHz power ultrasonic vibration 6min,
Obtain unit for uniform suspension;Rolling plate as negative electrode with standby surface modification magnesium alloy, carbon-point is anode, immerses and fills the above-mentioned gained of 190mL
In the electrolyzer of unit for uniform suspension, set electric field intensity as 5.6V/cm, electrophoretic deposition 50min, after electrophoretic deposition terminates, will
Cathode material is placed in 108 DEG C of baking ovens and is dried to constant weight, is proceeded to Muffle furnace subsequently, and under nitrogen guard mode, heating rises
Warm to 760 DEG C, sintering processes 1.5h, cool to room temperature with the furnace, obtain medical metal-based biological coating.
Gained of the present invention medical metal-based biological coating surface-brightening, without being mingled with, thickness is uniform, is 40 μm, interface cohesion
Intensity is 70MPa.
Example 3
Intercept a size of 20mm × 16mm × 1mm and roll plate AZ31 magnesium alloy, with abrasive paper for metallograph be polishing to surface uniform and smooth till,
Clean magnesium alloy with acetone and roll plate surface 5 times, then be 75% alcohol washes 4 times by mass concentration, after the natural air drying of surface, use
Hairbrush is through artificial coating 12g Mel, then magnesium alloy plate rolls plate proceeds in 80 DEG C of vacuum drying ovens, and dried 4h obtains pre-place
Reason magnesium alloy rolls plate, standby;In batch mixer, it is sequentially added into 4L sea water and 150g second pond activated sludge, starts and stir it, with
800r/min rotating speed stirring mixing 30min, discharging, gained material is proceeded in closed glass container, then glass container is placed in
Under sunlight, be exposed to the sun 5h;Wait end of being exposed to the sun, standby pretreatment magnesium alloy is rolled plate and puts in above-mentioned glass container, be placed in the sun
Under light, airtight process 5 weeks of being exposed to the sun, take out, be washed with deionized 5 times, remove magnesium alloy and roll plate remained on surface mud, then by magnesium
Alloy rolls plate and proceeds in 85 DEG C of vacuum drying ovens, dried 5h;Magnesium alloy after above-mentioned dry end is rolled plate and puts into Muffle
Stove, is passed through nitrogen with 5mL/min speed, until discharging all air, is progressively warming up to 440 DEG C with 6 DEG C/min speed subsequently,
Heat preservation sintering 30min under nitrogen guard mode, stops heating, cools to room temperature with the furnace, obtain surface modification magnesium alloy and roll plate, standby
With;In beaker, being sequentially added into 30g600 mesh hydroxyapatite powder, 220mL mass concentration is 75% ethanol solution, drips matter
Amount concentration is 12% ammonia, regulates pH to 9.0, then is proceeded to by beaker in sonic oscillation instrument, with 12kHz power ultrasonic vibration 8min,
Obtain unit for uniform suspension;Rolling plate as negative electrode with standby surface modification magnesium alloy, carbon-point is anode, immerses and fills the above-mentioned gained of 200mL
In the electrolyzer of unit for uniform suspension, set electric field intensity as 5.8V/cm, electrophoretic deposition 60min, after electrophoretic deposition terminates, will
Cathode material is placed in 110 DEG C of baking ovens and is dried to constant weight, is proceeded to Muffle furnace subsequently, and under nitrogen guard mode, heating rises
Warm to 780 DEG C, sintering processes 2h, cool to room temperature with the furnace, obtain medical metal-based biological coating.
Gained of the present invention medical metal-based biological coating surface-brightening, without being mingled with, thickness is uniform, is 50 μm, interface cohesion
Intensity is 72MPa.
Claims (1)
1. the preparation method of a medical metal-based biological coating, it is characterised in that concrete preparation process is:
(1) intercept a size of 20mm × 16mm × 1mm and roll plate AZ31 magnesium alloy, be polishing to abrasive paper for metallograph that surface is uniform and smooth is
Only, clean magnesium alloy with acetone and roll plate surface 3~5 times, then be 75% alcohol washes 2~4 times by mass concentration, treat that surface is natural
After Feng Ganing, with hairbrush through artificial coating 10~12g Mel, then magnesium alloy plate rolled plate proceed in 75~80 DEG C of vacuum drying ovens,
Dried 2~4h, obtains pretreatment magnesium alloy and rolls plate, standby;
(2) in batch mixer, it is sequentially added into 2~4L sea water and 100~150g second pond activated sludge, starts and stir it, with 600
~800r/min rotating speed stirring mixing 20~30min, discharging, gained material is proceeded in closed glass container, then glass is held
Device is placed under sunlight, is exposed to the sun 3~5h;
(3) wait end of being exposed to the sun, step (1) standby pretreatment magnesium alloy is rolled plate and puts in above-mentioned glass container, be placed in sunlight
Under, airtight process 3~5 weeks of being exposed to the sun, take out, be washed with deionized 3~5 times, remove magnesium alloy and roll plate remained on surface mud, then
Magnesium alloy is rolled plate and proceeds in 80~85 DEG C of vacuum drying ovens, dried 3~5h;
(4) magnesium alloy after above-mentioned dry end is rolled plate and puts into Muffle furnace, be passed through nitrogen with 3~5mL/min speed, until row
Go out all air, be progressively warming up to 400~440 DEG C with 4~6 DEG C/min speed subsequently, heat preservation sintering under nitrogen guard mode
20~30min, stop heating, cool to room temperature with the furnace, obtain surface modification magnesium alloy and roll plate, standby;
(5) in beaker, being sequentially added into 20~30g600 mesh hydroxyapatite powders, 200~220mL mass concentrations are 75% second
Alcoholic solution, dropping mass concentration is 8~12% ammonia, regulates pH to 8.8~9.0, then is proceeded to by beaker in sonic oscillation instrument, with
10~12kHz power ultrasonic vibrations 5~8min, obtain unit for uniform suspension;
(6) rolling plate as negative electrode with step (4) standby surface modification magnesium alloy, carbon-point is anode, immerses and fills on 180~200mL
State in the electrolyzer of gained unit for uniform suspension, set electric field intensity as 5.2~5.8V/cm, electrophoretic deposition 40~60min, treat electricity
After swimming deposition terminates, cathode material is placed in 105~110 DEG C of baking ovens and is dried to constant weight, proceeded to Muffle furnace subsequently, at nitrogen
Under gas shielded state, it is heated to 720 ~ 780 DEG C, sintering processes 1 ~ 2h, cool to room temperature with the furnace, obtain medical metal-based life
Thing coating.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610636146.4A CN106283160B (en) | 2016-08-05 | 2016-08-05 | A kind of preparation method of medical metal-based biological coating |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610636146.4A CN106283160B (en) | 2016-08-05 | 2016-08-05 | A kind of preparation method of medical metal-based biological coating |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106283160A true CN106283160A (en) | 2017-01-04 |
CN106283160B CN106283160B (en) | 2018-09-25 |
Family
ID=57664920
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610636146.4A Active CN106283160B (en) | 2016-08-05 | 2016-08-05 | A kind of preparation method of medical metal-based biological coating |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106283160B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107557783A (en) * | 2017-08-31 | 2018-01-09 | 常州富思通管道有限公司 | A kind of preparation method of composite medical magnesium alloy |
CN109999228A (en) * | 2019-02-28 | 2019-07-12 | 常州诺丁精密机械制造有限公司 | A kind of preparation method of strong corrosion resistant type magnesium alloy Biocomposite material |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1834306A (en) * | 2006-02-22 | 2006-09-20 | 福建师范大学 | Method of preparing electrophoretic deposited hydroxyl apatite coating on Ti or Ti alloy surface |
CN101254314A (en) * | 2007-03-02 | 2008-09-03 | 北京奥精医药科技有限公司 | Hydroxylapatite coating magnesium alloy medical inner implantation material and method of preparing the same |
WO2008146113A2 (en) * | 2007-05-28 | 2008-12-04 | Fin-Ceramica Faenza S.P.A. | Process for coating a surface of a metal element to increase osteointegration thereof and prosthetic device including said element |
US20100198345A1 (en) * | 2006-06-20 | 2010-08-05 | The University Of British Columbia | Calcium phosphate coated implantable medical devices, and electrophoretic deposition processes for making same |
CN102614545A (en) * | 2012-03-15 | 2012-08-01 | 河南师范大学 | Metal-based implant ternary compound coating material and preparation method thereof |
-
2016
- 2016-08-05 CN CN201610636146.4A patent/CN106283160B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1834306A (en) * | 2006-02-22 | 2006-09-20 | 福建师范大学 | Method of preparing electrophoretic deposited hydroxyl apatite coating on Ti or Ti alloy surface |
US20100198345A1 (en) * | 2006-06-20 | 2010-08-05 | The University Of British Columbia | Calcium phosphate coated implantable medical devices, and electrophoretic deposition processes for making same |
CN101254314A (en) * | 2007-03-02 | 2008-09-03 | 北京奥精医药科技有限公司 | Hydroxylapatite coating magnesium alloy medical inner implantation material and method of preparing the same |
WO2008146113A2 (en) * | 2007-05-28 | 2008-12-04 | Fin-Ceramica Faenza S.P.A. | Process for coating a surface of a metal element to increase osteointegration thereof and prosthetic device including said element |
CN102614545A (en) * | 2012-03-15 | 2012-08-01 | 河南师范大学 | Metal-based implant ternary compound coating material and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107557783A (en) * | 2017-08-31 | 2018-01-09 | 常州富思通管道有限公司 | A kind of preparation method of composite medical magnesium alloy |
CN109999228A (en) * | 2019-02-28 | 2019-07-12 | 常州诺丁精密机械制造有限公司 | A kind of preparation method of strong corrosion resistant type magnesium alloy Biocomposite material |
Also Published As
Publication number | Publication date |
---|---|
CN106283160B (en) | 2018-09-25 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103751840B (en) | A kind of have bone defect repair support of the controlled low modulus of porous and preparation method thereof | |
Seyedraoufi et al. | Effects of pulse electrodeposition parameters and alkali treatment on the properties of nano hydroxyapatite coating on porous Mg–Zn scaffold for bone tissue engineering application | |
CN104674320A (en) | Preparation method and application of wear-resistant antibacterial bioactive ceramic film for titanium or titanium alloy surface | |
Jemat et al. | Effects of TiO2 on microstructural, mechanical properties and in-vitro bioactivity of plasma sprayed yttria stabilised zirconia coatings for dental application | |
CN101560685B (en) | Method for preparing bioactive coating on titanium alloy surface | |
CN102793947B (en) | Degradable magnesium and surface modification method of alloy thereof | |
CN102409382A (en) | Bioactive coating of metal implant and preparation method thereof | |
CN100430099C (en) | Bioactive coating on surface of Titanium or titanium alloy and its preparing method | |
CN106011815A (en) | Preparation method for hybrid composite coating used for magnesium-based biological material surface medication | |
CN103668397B (en) | A kind of high-activity biological gradient cladding for titanium alloy surface | |
CN106283160A (en) | A kind of preparation method of medical metal-based biological coating | |
CN102113918A (en) | Method for preparing porous structure on surface of pure titanium dental implant | |
CN101455859B (en) | Titanium alloy surface Ti-YSZ-FHA biological gradient active coatings and preparation method thereof | |
CN101342387A (en) | Activation method for quickly generating phosphatic rock on titanium coating surface | |
CN108004527A (en) | A kind of preparation method of zinc doping hydroxyapatite coating layer for magnesium alloy materials | |
JP4425198B2 (en) | Calcium titanate / amorphous carbon composite, coating material using the same, and method for producing the same | |
CN108273134A (en) | A kind of preparation method of antibacterial magnesium-based biological coating | |
CN103446626B (en) | Medical degradable bioglass/phytic acid composite coating on surface of magnesium alloy and preparation method thereof | |
CN105603484B (en) | A kind of coating and preparation method thereof that can improve medical magnesium and Mg alloy surface corrosion resistance and biocompatibility | |
CN105543934A (en) | Medical titanium implant micro-arc oxidation film layer and preparation method | |
CN102286764A (en) | Method for preparing periodical absorbable Hyaluronic Acid/acyl carrier protein (HA/ACP) composite coating on titanium implant surface | |
CN108103551B (en) | A kind of method of hydroxylapatite crystal in promotion differential arc oxidation film layer | |
CN104707170B (en) | Titanium surface prepares nano-grade hydroxy apatite layer load rapamycin drug method | |
Zhao et al. | Effects of temperature and voltage on formation of electrolysis induced chemical conversion coating on titanium surface | |
CN108517515A (en) | The method for preparing Mg alloy surface zinc doping calcium phosphor coating using one step hydro thermal method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
TA01 | Transfer of patent application right | ||
TA01 | Transfer of patent application right |
Effective date of registration: 20180821 Address after: 322100 Zhejiang, Jinhua, Dongyang, Jiangbei street, 1 New Village Applicant after: New Mstar Technology Ltd in Dongyang Address before: 315000 room 651, Sang Tian Road, Jiangdong District, Ningbo, Zhejiang, 651 Applicant before: NINGBO JIANGDONG LUNSIFU ENVIRONMENTAL PROTECTION TECHNOLOGY CO., LTD. |
|
GR01 | Patent grant | ||
GR01 | Patent grant |