CN105903075A - Preparation method of Ca-P based bio-coating on carbon/carbon matrix surface - Google Patents
Preparation method of Ca-P based bio-coating on carbon/carbon matrix surface Download PDFInfo
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- CN105903075A CN105903075A CN201610374648.4A CN201610374648A CN105903075A CN 105903075 A CN105903075 A CN 105903075A CN 201610374648 A CN201610374648 A CN 201610374648A CN 105903075 A CN105903075 A CN 105903075A
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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
- A61L27/32—Phosphorus-containing materials, e.g. apatite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/08—Carbon ; Graphite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- 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
Abstract
The invention discloses a preparation method of a Ca-P based bio-coating on a carbon/carbon matrix surface to solve the technical problem of poor bonding strength between bio-coatings prepared by exiting methods and matrixes. The technical scheme includes: dissolving calcium carbonate and diammonium hydrogen phosphate in deionized water and conducting stirring to form a calcium-phosphorus solution, impregnating a carbon/carbon matrix in the calcium-phosphorus solution, putting the solution into a microwave reaction kettle to carry out reaction, thus generating a layer of Ca-P based bio-coating on the carbon/carbon composite material surface, performing supersonic plasma spraying of hydroxyapatite powder on the carbon/carbon matrix subjected to microwave hydrothermal treatment, then conducting natural cooling to room temperature so as to obtain the Ca-P based bio-coating on the carbon/carbon composite material surface. The method provided by the invention combines microwave hydrothermal process with supersonic plasma spraying process, the prepared Ca-P based bio-coating undergoes in-situ growth from the carbon/carbon composite material surface, the Ca-P based bio-coating combines with the carbon/carbon matrix in a rough dentation manner, thereby improving the bonding strength of the bio-coating and the matrix.
Description
Technical field
The invention belongs to carbon/carbon composite field, particularly to a kind of charcoal/carbon matrix surface C a-P base biological coating
Preparation method.
Background technology
Carbon/carbon composite is with carbon fiber for strengthening the C-base composte material of phase, and it forms all carbons, is a kind of
Have both the novel high-performance composite of 26S Proteasome Structure and Function characteristic, belong to inert material, there is density low (generally less than
2.0g/cm3), geometrical stability x radiation x strong, resistance to, good biocompatibility, X ray image is without artifact, springform
Amount is near with people's bone photo, can effectively avoid " stress shielding " effect.Have the mechanical property that fibre reinforced materials is excellent concurrently
The biocompatibility good with carbonaceous material.Additionally, carbon/carbon composite has open space bone, tissue is the longest
Enter wherein.Therefore, carbon/carbon compound material is a kind of artificial bone biology material with applications well prospect at field of orthopaedics
Material.But, carbon/carbon composite is applied to biomedical sector, still suffers from problems with: (1) prepares skill from material
Analyzing in art, existing carbon/carbon composite is mainly aerospace field application, and lacks of bio-medical field and answer
Carbon/carbon composite structure design.Should from bio-medical angle, according to the true form of skeleton,
Size and stress distribution situation, design precursor structure, prepare the special carbon/carbon composite of human bone joint replacement；(2)
Analyzing from the characteristic of carbonaceous material, carbon/carbon composite belongs to bio-inert material, itself does not have biological activity,
Need it to be carried out surface bioactive process, to be preferably applied for clinic；(3) carbon/carbon composite implant circle
The release of carbon particulate is caused because of friction, although preliminary study reference soma is not encroached on by carbon particulate at face,
But for the stability of implant and the impact of avoiding the unknown, should manage to reduce wear particle.Therefore, composite
Matrix surface must carry out matrix modification.
Bioactive materials includes hydroxyapatite (HA), tricalcium phosphate (TCP), calcium hydrogen phosphate (ADCP) etc.,
It is that human bone repairs main component.Wherein, hydroxyapatite is the main inorganic composition in vertebrate skeletal and tooth,
There is chemical composition and crystal structure that in skeleton and tooth, main mine material is similar, account in people's tooth 95% with
On, the content of people's bone is also above 60%.Chemical combination bond can be organized the formation of with skeleton to close, nontoxic in implanting human body,
Harmless, without carcinogenesis, and there is good biocompatibility and biological activity, be a kind of typical biomaterial.
Therefore hydroxylapatite ceramic is widely used in the reparation of osseous tissue defect.But due to simple hydroxylapatite ceramic power
Learning poor-performing, its bending strength and fracture toughness index are below human body compact bone, so being difficult to carry at organism
Position uses.
The preparation method of carbon/carbon composite surface C a-P base biological coating mainly has: Biomimetic, plasma spray
Coating, electrophoresis method, electrochemical deposition method, microwave-hydrothermal method etc., wherein Biomimetic is that sedimentation time is longer；Electricity
Swimming method is by Electrostatic Absorption rather than metallurgical absorption or chemical bond between microgranule and matrix, thus coating and matrix
Bond strength is the highest；The adhesion of coating and matrix surface that electrochemical deposition method obtains is poor.
Document 1 " Jin-Ling Sui, Mu-Sen Li, Long-Wei Yin, Yun-Jing Song.Plasma-sprayed
hydroxyapatite coatings on carbon/carbon composites.Surface and Coatings Technology
176 (2004) 188-192. " disclose a kind of method of Supersonic Plasma Spraying and prepare hydroxylapatite biology and be coated with
Layer, the anchoring strength of coating that the method is only prepared with single spraying method is poor, easy to fall off.
Document 2 Chinese invention patent of CN101584881A " application publication number be " discloses a kind of compound hydroxy-apatite
Stone coating and preparation method thereof, belongs to bio-medical material artificial growth association area.The preparation process of this composite coating
It is to be respectively adopted microplasma spraying equipment by hydroxyapatite powder sprayed layer undercoat and spraying on bottom on matrix
Surface layer.The method is only the simple introduction to a kind of plasma spraying hydroxyapatite, though utilizing two step plasma spray
It is coated with, but powder consumption is big, and single hydroxyapatite coating layer is difficult to meet the requirement in bio-medical field, in conjunction with strong
Spending the highest, its shear strength only has 2.0MPa.
Summary of the invention
In order to overcome the deficiency of biological coating prepared by existing method and substrate combinating strength difference, the present invention provide a kind of charcoal/
The preparation method of carbon matrix surface C a-P base biological coating.Calcium carbonate and diammonium phosphate are dissolved in deionized water by the method
In and stir formation calcium phosphorus solution, treated charcoal/carbon matrix is immersed in calcium phosphorus solution, puts into microwave reaction kettle
Middle reaction, at one layer of Ca-P base biological coating of carbon/carbon composite Surface Creation.To the charcoal processed through microwave hydrothermal/
Carbon matrix carries out Supersonic Plasma Spraying hydroxyapatite powder, and spraying terminates, and naturally cools to room temperature, charcoal/
Carbon composite surface obtains Ca-P base biological coating.The present invention is by microwave-hydrothermal method and Supersonic Plasma Spraying method
Combine, the Ca-P base biological coating of preparation from carbon/carbon composite surface in situ grow, Ca-P base biological coating in
Indenting shape is combined with charcoal/carbon matrix, improves biological coating and substrate combinating strength.
The technical solution adopted for the present invention to solve the technical problems: a kind of charcoal/carbon matrix surface C a-P base biological coating
Preparation method, be characterized in comprising the following steps:
Step one, the calcium carbonate of 0.167-1.670mol/L and the diammonium phosphate of 0.100-1.000mol/L are dissolved in from
In sub-water, stirring with magnetic stirring apparatus, form calcium phosphorus solution, the charcoal/carbon matrix then polishing cleaned is complete
Entirely it is immersed in calcium phosphorus solution, puts in microwave reaction kettle, the temperature of microwave hydrothermal is arranged on 90-120 DEG C, the time
For 5-30min.Question response takes out after terminating, and at one layer of Ca-P base biological coating of carbon/carbon composite Surface Creation, uses
Deionized water rinsing removes the not long Ca-P base biological coating powder on charcoal/carbon matrix of material surface attachment, dries
Standby.
Step 2, the charcoal/carbon matrix processed through step one microwave hydrothermal is carried out Supersonic Plasma Spraying, spray grain
Footpath is the hydroxyapatite powder of 75-150 μm, is sprayed on the matrix after microwave hydrothermal processes, spraying coating process
Parameter is: operating current is 330-380A；Spray distance is 100-150mm；Spraying number of times 10-20 time；Carrier gas stream
Amount 70-80L/min；Secondary air flow 2.0-3.0L/min；Powder sending quantity 4.0-5.2g/min.Spraying terminates, the coldest
But to room temperature, Ca-P base biological coating is obtained on carbon/carbon composite surface.
The invention has the beneficial effects as follows: calcium carbonate and diammonium phosphate are dissolved in deionized water and stir formation by the method
Calcium phosphorus solution, is immersed in treated charcoal/carbon matrix in calcium phosphorus solution, puts in microwave reaction kettle and reacts, at charcoal
One layer of Ca-P base biological coating of/carbon composite Surface Creation.Charcoal/the carbon matrix processed through microwave hydrothermal is surpassed
Velocity of sound plasma spraying hydroxyapatite powder, spraying terminates, and naturally cools to room temperature, on carbon/carbon composite surface
Obtain Ca-P base biological coating.Microwave-hydrothermal method is combined by the present invention with Supersonic Plasma Spraying method, preparation
Ca-P base biological coating grows from carbon/carbon composite surface in situ, Ca-P base biological coating in indenting shape with charcoal/
Carbon matrix combines, and improves biological coating and substrate combinating strength.After tested, the shearing that biological coating is combined with matrix
Intensity is brought up to 8.21MPa by the 2.0MPa of background technology.
With detailed description of the invention, the present invention is elaborated below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is the surface topography SEM picture of the Ca-P base biological coating of the inventive method embodiment 4 preparation.
Fig. 2 is the EDS spectrogram of the Ca-P base composite biological coating of the inventive method embodiment 4 preparation.
Fig. 3 is the XRD figure of the Ca-P base biological coating of the inventive method embodiment 4 preparation.
Detailed description of the invention
Following example are with reference to Fig. 1-3.
Embodiment 1.
The calcium carbonate of 0.167mol/L and the diammonium phosphate of 0.100mol/L are dissolved in deionized water, use magnetic stirring apparatus
Stir, then charcoal/carbon matrix that polishing is cleaned is completely infused in calcium phosphorus solution, puts into microwave reaction
In still, the temperature of microwave hydrothermal being arranged on 90 DEG C, the time is 30min.Question response takes out after terminating, multiple at charcoal/charcoal
One layer of Ca-P base biological coating of condensation material Surface Creation, washes not growing at charcoal except material surface attachment with deionized water
Ca-P base biological coating powder on/carbon matrix, dry for standby.
Existing hydroxyapatite powder is reached 75 μm that spraying requires, fixing base by pelletize, then sprays
Being coated with, spraying parameter is: operating current is 330A；Spray distance is 100mm；Spraying number of times 10 times；Carrier gas
Flow 70L/min；Secondary air flow 2.0L/min；Powder sending quantity 5.2g/min.Spraying terminates, and naturally cools to room temperature,
Composite biological coating is obtained on carbon/carbon composite surface.
After tested, the shear strength that the biological coating that the present embodiment is prepared on carbon/carbon composite surface is combined with matrix is
8.21MPa。
Embodiment 2.
The calcium carbonate of 0.501mol/L and the diammonium phosphate of 0.300mol/L are dissolved in deionized water, use magnetic stirring apparatus
Stir, then charcoal/carbon matrix that polishing is cleaned is completely infused in calcium phosphorus solution, puts into microwave reaction
In still, the temperature of microwave hydrothermal being arranged on 100 DEG C, the time is 20min.Question response takes out after terminating, at charcoal/charcoal
Composite material surface generates one layer of Ca-P base biological coating, washes not growing except material surface attachment with deionized water
Ca-P base biological coating powder on charcoal/carbon matrix, dry for standby.
Existing hydroxyapatite powder is reached 100 μm that spraying requires, fixing base by pelletize, then carries out
Spraying, spraying parameter is: operating current is 350A；Spray distance is 120mm；Spraying number of times 13 times；Carry
Throughput 73L/min；Secondary air flow 2.3L/min；Powder sending quantity 5.0g/min.Spraying terminates, and naturally cools to room
Temperature, obtains composite biological coating on carbon/carbon composite surface.
Embodiment 3.
The calcium carbonate of 1.002mol/L and the diammonium phosphate of 0.600mol/L are dissolved in deionized water, use magnetic stirring apparatus
Stir, then charcoal/carbon matrix that polishing is cleaned is completely infused in calcium phosphorus solution, puts into microwave reaction
In still, the temperature of microwave hydrothermal being arranged on 110 DEG C, the time is 15min.Question response takes out after terminating, at charcoal/charcoal
Composite material surface generates one layer of Ca-P base biological coating, washes not growing except material surface attachment with deionized water
Ca-P base biological coating powder on charcoal/carbon matrix, dry for standby.
Existing hydroxyapatite powder is reached 125 μm that spraying requires, fixing base by pelletize, then carries out
Spraying, spraying parameter is: operating current is 370A；Spray distance is 130mm；Spraying number of times 16 times；Carry
Throughput 76L/min；Secondary air flow 2.6L/min；Powder sending quantity 4.5g/min.Spraying terminates, and naturally cools to room
Temperature, obtains composite biological coating on carbon/carbon composite surface.
Embodiment 4.
The calcium carbonate of 1.670mol/L and the diammonium phosphate of 1.000mol/L are dissolved in deionized water, use magnetic stirring apparatus
Stir, then charcoal/carbon matrix that polishing is cleaned is completely infused in calcium phosphorus solution, puts into microwave reaction
In still, the temperature of microwave hydrothermal being arranged on 120 DEG C, the time is 5min.Question response takes out after terminating, multiple at charcoal/charcoal
One layer of Ca-P base biological coating of condensation material Surface Creation, washes not growing at charcoal except material surface attachment with deionized water
Ca-P base biological coating powder on/carbon matrix, dry for standby.
Existing hydroxyapatite powder is reached 150 μm that spraying requires, fixing base by pelletize, then carries out
Spraying, spraying parameter is: operating current is 380A；Spray distance is 150mm；Spraying number of times 20 times；Carry
Throughput 80L/min；Secondary air flow 3.0L/min；Powder sending quantity 4.0g/min.Spraying terminates, and naturally cools to room
Temperature, obtains composite biological coating on carbon/carbon composite surface.
From figure 1 it appears that Ca-P base biological coating prepared by the present embodiment has table interlocking, coarse
Face pattern, and it is tiny to be evenly distributed, and produces mutually without other impurity, produces excellence with Supersonic Plasma Spraying coating
Conjugation condition.
From figure 2 it can be seen that Ca, P ratio in the Ca-P base biological coating prepared of the present embodiment, miscellaneous without other
Prime element.
From figure 3, it can be seen that Ca-P base biological coating crystal property prepared by the present embodiment is excellent and miscellaneous without other
Matter phase.
Claims (1)
1. the preparation method of charcoal/carbon matrix surface C a-P base biological coating, it is characterised in that comprise the following steps:
Step one, the calcium carbonate of 0.167-1.670mol/L and the diammonium phosphate of 0.100-1.000mol/L are dissolved in from
In sub-water, stirring with magnetic stirring apparatus, form calcium phosphorus solution, the charcoal/carbon matrix then polishing cleaned is complete
Entirely it is immersed in calcium phosphorus solution, puts in microwave reaction kettle, the temperature of microwave hydrothermal is arranged on 90-120 DEG C, the time
For 5-30min；Question response takes out after terminating, and at one layer of Ca-P base biological coating of carbon/carbon composite Surface Creation, uses
Deionized water rinsing removes the not long Ca-P base biological coating powder on charcoal/carbon matrix of material surface attachment, dries
Standby；
Step 2, the charcoal/carbon matrix processed through step one microwave hydrothermal is carried out Supersonic Plasma Spraying, spray grain
Footpath is the hydroxyapatite powder of 75-150 μm, is sprayed on the matrix after microwave hydrothermal processes, spraying coating process
Parameter is: operating current is 330-380A；Spray distance is 100-150mm；Spraying number of times 10-20 time；Carrier gas stream
Amount 70-80L/min；Secondary air flow 2.0-3.0L/min；Powder sending quantity 4.0-5.2g/min；Spraying terminates, the coldest
But to room temperature, Ca-P base biological coating is obtained on carbon/carbon composite surface.
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| CN201610374648.4A CN105903075B (en) | 2016-05-31 | 2016-05-31 | Charcoal/carbon matrix surface C a-P base biological coating preparation method |
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| CN201610374648.4A CN105903075B (en) | 2016-05-31 | 2016-05-31 | Charcoal/carbon matrix surface C a-P base biological coating preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108998819A (en) * | 2018-05-29 | 2018-12-14 | 深圳大学 | The preparation method of microwave hydrothermal electro-deposition system and calcium phosphorus biological coating |
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| WO2009147469A1 (en) * | 2008-06-03 | 2009-12-10 | Lechler S.P.A. | Water- based coating composition containing dialkyl carbonates having ether functions as coalescent agents and use therof |
| CN103498183A (en) * | 2013-10-17 | 2014-01-08 | 赵全明 | Preparation technology of hydroxyapatite-containing composite biological film on titanium-base surface |
| CN103961745A (en) * | 2014-05-14 | 2014-08-06 | 常州大学 | Method of quickly preparing calcium phosphate coating containing third-party beneficial ions |
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2016
- 2016-05-31 CN CN201610374648.4A patent/CN105903075B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009147469A1 (en) * | 2008-06-03 | 2009-12-10 | Lechler S.P.A. | Water- based coating composition containing dialkyl carbonates having ether functions as coalescent agents and use therof |
| CN103498183A (en) * | 2013-10-17 | 2014-01-08 | 赵全明 | Preparation technology of hydroxyapatite-containing composite biological film on titanium-base surface |
| CN103961745A (en) * | 2014-05-14 | 2014-08-06 | 常州大学 | Method of quickly preparing calcium phosphate coating containing third-party beneficial ions |
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| CN108998819A (en) * | 2018-05-29 | 2018-12-14 | 深圳大学 | The preparation method of microwave hydrothermal electro-deposition system and calcium phosphorus biological coating |
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