CN107326338B - A method of realizing that carbon nanotube is evenly dispersed in Ca-P base biological coating - Google Patents

A method of realizing that carbon nanotube is evenly dispersed in Ca-P base biological coating Download PDF

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CN107326338B
CN107326338B CN201710469681.XA CN201710469681A CN107326338B CN 107326338 B CN107326338 B CN 107326338B CN 201710469681 A CN201710469681 A CN 201710469681A CN 107326338 B CN107326338 B CN 107326338B
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carbon nanotube
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CN107326338A (en
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李贺军
刘守杰
张磊磊
孙佳佳
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Northwestern Polytechnical University
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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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • 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
    • A61L27/303—Carbon
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/18—Electroplating using modulated, pulsed or reversing current
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54—Electroplating of non-metallic surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • 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
    • A61L2420/00—Materials or methods for coatings medical devices
    • A61L2420/04—Coatings containing a composite material such as inorganic/organic, i.e. material comprising different phases
    • 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 present invention relates to a kind of to realize the evenly dispersed method of carbon nanotube in Ca-P base biological coating, by after surface of carbon/carbon composite pulse electrodeposition Ca-P base biological coating, pulse electrodeposition processing is carried out again to it, it is dispersed in catalyst iron in Ca-P base biological coating, then using dimethylbenzene as carbon source, ethylenediamine is growth regulator, and chemical vapor carbon deposition nanotube is final to realize that carbon nanotube is evenly dispersed in Ca-P base biological coating.The utility model has the advantages that carbon nanotube is uniformly applied in the composite coating by Ca-P biological coating, ultimately forming evenly dispersed carbon nanotube with being combined closely by Ca-P biological coating.

Description

A method of realizing that carbon nanotube is evenly dispersed in Ca-P base biological coating
Technical field
The invention belongs to technical field of biological material, are related to one kind and realize that carbon nanotube is evenly dispersed in Ca-P base biological coating Method.
Background technique
Ca-P base ceramic material is similar with the inorganic matter in skeleton, has excellent bioactivity and bio-compatible Property, it is often compound with metal material, nonmetallic materials and polymer material, as can load-bearing can induce the life of bone tissue regeneration again Object alternate material.Preparation carbon nanotube enhancing Ca-P coating is mainly first to mix carbon nanotube with Ca-P powder machinery at present Afterwards, re-coating is in matrix surface.This method not can effectively solve that carbon nanotube disperses unevenness in Ca-P base biomaterial The problem of, and also will cause different degrees of damage to carbon nanotube.
Document 1 " Y.Chen, Y.Q.Zhang, T.H.Zhang, C.H.Gan, C.Y.Zheng, G.Yu.Carbon nanotube reinforced hydroxyapatite composite coatings produced through laser Surface alloying.Carbon 44 (2006) 37-45. " reports mechanical mixture carbon nanotube and hydroxy apatite powder Afterwards, carbon nano-tube reinforced hydroxylapatite composite coating is prepared in titanium alloy surface using laser surface alloying method.As a result Show that content of carbon nanotubes is more, disperses uneven phenomenon and be more obvious.
" Y.H.Meng, C.Y.Tang, C.P.Tsui.Fabrication and the characterization of of document 2 needle-like nano-HA and HA/MWCNT composites.Journal of Materials Science: It can be a kind of improvement carbon nanotube point that Materials in Medicine 19 (2008) 75-81. ", which is reported and handled using soda acid, Dissipate a kind of method of property.Still there is carbon nanotube problem easy to reunite in Ca-P biological coating.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that one kind realizes carbon nanometer in Ca-P base biological coating Evenly dispersed method is managed, solves the problems, such as that carbon nanotube is easy to reunite in Ca-P biological coating.
Technical solution
A method of realizing that carbon nanotube is evenly dispersed in Ca-P base biological coating, it is characterised in that steps are as follows:
Step 1: four water-calcium nitrate solution and ammonium dihydrogen phosphate being mixed in equal volume and are placed on pulse electrodeposition device In, using carbon/carbon composite material base body as cathode, graphite is deposited as anode, is obtained in surface of carbon/carbon composite Ca-P base biological coating is named as A；
Deposition process conditions are as follows: sedimentation time is 1.0-2.0h, and deposition voltage is 5.0-10.0V, depositing temperature 60-80 DEG C, pulse switching time ratio is 0.25-1.00；
The concentration of the four water-calcium nitrate solution is 1.67 × 10-2-1.67mol/L；
The concentration of the ammonium dihydrogen phosphate is 1.00 × 10-2-1.00mol/L；
Step 2: pulse electrodeposition processing will be carried out after A drying, realizes and introduce catalyst iron in Ca-P base biological coating, It is named as B；Pulse electrodeposition processing；
Pulse electrodeposition treatment process condition are as follows: six aqueous ferrous sulfate solution concentration of electrolyte is 0.02-2.00g/ml, is sunk Product time 0.5-1.5h, deposition voltage are 5.0-10.0V, and depositing temperature is 60-80 DEG C, and pulse switching time ratio is 0.25- 1.00；
Step 3: B is intracavitary as chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, realize Carbon nanotube is evenly dispersed in Ca-P base biological coating；
The technique of deposition of carbon nanotubes are as follows: at 400-600 DEG C after hydrogen reducing catalyst iron, at 750-900 DEG C, argon Under the conditions of gas, hydrogen flowing quantity are respectively 400 and 200sccm, using dimethylbenzene as carbon source, ethylenediamine is growth regulator, injection rate ratio It is 5.0-10.0, injection time 0.5-2h.
Beneficial effect
It is proposed by the present invention it is a kind of the evenly dispersed method of carbon nanotube is realized in Ca-P base biological coating, by After surface of carbon/carbon composite pulse electrodeposition Ca-P base biological coating, pulse electrodeposition processing is carried out to it again, makes catalyst Iron is dispersed in Ca-P base biological coating, and then using dimethylbenzene as carbon source, ethylenediamine is growth regulator, chemical vapor carbon deposition Nanotube, it is final to realize that carbon nanotube is evenly dispersed in Ca-P base biological coating.Superiority: from figure 1 it appears that this reality It applies example and prepares catalyst iron and be dispersed in porous C a-P biological coating.Calcium, phosphorus, oxygen and ferro element are distributed in the coating in figure Situation, wherein calcium, phosphorus, oxygen element are Ca-P biological coating components, and ferro element is the catalyst iron obtained after electro-deposition.From In Fig. 2 as can be seen that carbon nanotube be uniformly applied in by Ca-P biological coating, ultimately form evenly dispersed carbon nanotube with The composite coating combined closely by Ca-P biological coating.
Detailed description of the invention
Fig. 1 is the energy spectrum diagram of electro-deposition catalyst iron in porous C a-P biological coating of embodiment of the present invention method 4.
Fig. 2 is the scanning electricity of original position deposition of carbon nanotubes in porous C a-P biological coating of embodiment of the present invention method 4 Mirror picture.
Specific embodiment
Now in conjunction with embodiment, attached drawing, the invention will be further described:
Embodiment 1:
It is respectively 1.67 × 10 by concentration-2The four water-calcium nitrate solution of mol/L and 1.00 × 10-2The biphosphate of mol/L Ammonium salt solution uniformly mixes in equal volume, and then using carbon/carbon composite material base body as cathode, graphite is placed in pulse electricity as anode In precipitation equipment, sedimentation time 1.5h, deposition voltage 5V, depositing temperature are 70 DEG C, and pulse switching time ratio is 1.00. The Ca-P base biological coating that will be obtained in surface of carbon/carbon composite, is named as A；
After A drying, pulse electrodeposition processing, process conditions are as follows: six aqueous ferrous sulfate solution concentration of electrolyte are carried out to A For 0.2g/ml, sedimentation time 1h, deposition voltage 5V, depositing temperature is 70 DEG C, and pulse switching time ratio is 1.00.To real Catalyst iron is introduced in present Ca-P base biological coating, is named as B；
It is intracavitary that B is placed in chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, depositing operation are as follows: At 400 DEG C after hydrogen reducing catalyst iron, at 750 DEG C, under the conditions of argon gas, hydrogen flowing quantity are respectively 400 and 200sccm, with Dimethylbenzene is carbon source, and ethylenediamine is growth regulator, and injection rate ratio is 5.0, injection time 0.5h.It is final to realize in the life of Ca-P base Carbon nanotube is evenly dispersed in object coating.
Embodiment 2:
It is respectively 1.67 × 10 by concentration-1The four water-calcium nitrate solution of mol/L and 1.00 × 10-1The biphosphate of mol/L Ammonium salt solution uniformly mixes in equal volume, and then using carbon/carbon composite material base body as cathode, graphite is placed in pulse electricity as anode In precipitation equipment, sedimentation time 1.5h, deposition voltage 7.5V, depositing temperature are 80 DEG C, and pulse switching time ratio is 0.50.The Ca-P base biological coating that will be obtained in surface of carbon/carbon composite, is named as A；
After A drying, pulse electrodeposition processing, process conditions are as follows: six aqueous ferrous sulfate solution concentration of electrolyte are carried out to A For 2g/ml, sedimentation time 0.5h, deposition voltage 7.5V, depositing temperature is 80 DEG C, and pulse switching time ratio is 0.50.To It realizes and introduces catalyst iron in Ca-P base biological coating, be named as B；
It is intracavitary that B is placed in chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, depositing operation are as follows: At 450 DEG C after hydrogen reducing catalyst iron, at 800 DEG C, under the conditions of argon gas, hydrogen flowing quantity are respectively 400 and 200sccm, with Dimethylbenzene is carbon source, and ethylenediamine is growth regulator, and injection rate ratio is 10, injection time 1h.It is final to realize in Ca-P base biology Carbon nanotube is uniformly distributed in coating.
Embodiment 3:
It is respectively the bodies such as the four water-calcium nitrate solution of 1.67mol/L and the ammonium dihydrogen phosphate of 1.00mol/L by concentration Product uniformly mixing, then using carbon/carbon composite material base body as cathode, graphite is placed in pulse electrodeposition device as anode In, sedimentation time 1h, deposition voltage 10V, depositing temperature are 60 DEG C, and pulse switching time ratio is 0.25.It will be in carbon/carbon The Ca-P base biological coating that composite material surface obtains is named as A；
After A drying, pulse electrodeposition processing, process conditions are as follows: six aqueous ferrous sulfate solution concentration of electrolyte are carried out to A For 0.02g/ml, sedimentation time 1.5h, deposition voltage 10V, depositing temperature is 60 DEG C, and pulse switching time ratio is 0.25.From And realize and introduce catalyst iron in Ca-P base biological coating, it is named as B；
It is intracavitary that B is placed in chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, depositing operation are as follows: At 500 DEG C after hydrogen reducing catalyst iron, at 900 DEG C, under the conditions of argon gas, hydrogen flowing quantity are respectively 400 and 200sccm, with Dimethylbenzene is carbon source, and ethylenediamine is growth regulator, and injection rate ratio is 5.0, injection time 1.5h.It is final to realize in the life of Ca-P base Carbon nanotube is evenly dispersed in object coating.
Embodiment 4:
It is respectively 1.67 × 10 by concentration-2The four water-calcium nitrate solution of mol/L and 1.00 × 10-2The biphosphate of mol/L Ammonium salt solution uniformly mixes in equal volume, and then using carbon/carbon composite material base body as cathode, graphite is placed in pulse electricity as anode In precipitation equipment, sedimentation time 2h, deposition voltage 10V, depositing temperature are 60 DEG C, and pulse switching time ratio is 0.25.It will A is named as in the Ca-P base biological coating that surface of carbon/carbon composite obtains；
After A drying, pulse electrodeposition processing is carried out to A.Process conditions are as follows: six aqueous ferrous sulfate solution concentration of electrolyte For 0.02g/ml, sedimentation time 0.5h, deposition voltage 10V, depositing temperature is 60 DEG C, and pulse switching time ratio is 0.25.From And realize and introduce catalyst iron in Ca-P base biological coating, it is named as B；
It is intracavitary that B is placed in chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, depositing operation are as follows: At 500 DEG C after hydrogen reducing catalyst iron, at 850 DEG C, under the conditions of argon gas, hydrogen flowing quantity are respectively 400 and 200sccm, with Dimethylbenzene is carbon source, and ethylenediamine is growth regulator, and injection rate ratio is 7.5, injection time 1h.It is final to realize in Ca-P base biology Carbon nanotube is evenly dispersed in coating.
Embodiment 5:
It is respectively 1.67 × 10 by concentration-1The four water-calcium nitrate solution of mol/L and 1.00 × 10-1The biphosphate of mol/L Ammonium salt solution uniformly mixes in equal volume, and then using carbon/carbon composite material base body as cathode, graphite is placed in pulse electricity as anode In precipitation equipment, sedimentation time 1h, deposition voltage 10V, depositing temperature are 60 DEG C, and pulse switching time ratio is 0.75.It will A is named as in the Ca-P base biological coating that surface of carbon/carbon composite obtains；
After A drying, pulse electrodeposition processing is carried out to A.Process conditions are as follows: six aqueous ferrous sulfate solution concentration of electrolyte For 0.2g/ml, sedimentation time 1h, deposition voltage 7.5V, depositing temperature is 60 DEG C, and pulse switching time ratio is 0.75.To It realizes and introduces catalyst iron in Ca-P base biological coating, be named as B；
It is intracavitary that B is placed in chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, depositing operation are as follows: At 600 DEG C after hydrogen reducing catalyst iron, at 900 DEG C, under the conditions of argon gas, hydrogen flowing quantity are respectively 400 and 200sccm, with Dimethylbenzene is carbon source, and ethylenediamine is growth regulator, and injection rate ratio is 5, injection time 0.5h.It is final to realize in Ca-P base biology Carbon nanotube is evenly dispersed in coating.
Embodiment 6:
It is respectively the bodies such as the four water-calcium nitrate solution of 1.67mol/L and the ammonium dihydrogen phosphate of 1.00mol/L by concentration Product uniformly mixing, then using carbon/carbon composite material base body as cathode, graphite is placed in pulse electrodeposition device as anode In, sedimentation time 2h, deposition voltage 7.5V, depositing temperature are 80 DEG C, and pulse switching time ratio is 1.00.It will be in carbon/carbon The Ca-P base biological coating that composite material surface obtains is named as A；
After A drying, pulse electrodeposition processing is carried out to A.Process conditions are as follows: six aqueous ferrous sulfate solution concentration of electrolyte For 2g/ml, sedimentation time 1h, deposition voltage 7.5V, depositing temperature is 60 DEG C, and pulse switching time ratio is 1.00.To real Catalyst iron is introduced in present Ca-P base biological coating, is named as B；
It is intracavitary that B is placed in chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, depositing operation are as follows: At 550 DEG C after hydrogen reducing catalyst iron, at 900 DEG C, under the conditions of argon gas, hydrogen flowing quantity are respectively 400 and 200sccm, with Dimethylbenzene is carbon source, and ethylenediamine is growth regulator, and injection rate ratio is 10, injection time 1.5h.It is final to realize in the life of Ca-P base Carbon nanotube is evenly dispersed in object coating.

Claims (1)

1. a kind of realize the evenly dispersed method of carbon nanotube in Ca-P base biological coating, it is characterised in that steps are as follows:
Step 1: four water-calcium nitrate solution and ammonium dihydrogen phosphate are mixed in equal volume and are placed in pulse electrodeposition device, with Carbon/carbon composite material base body is deposited as cathode, graphite as anode, in the Ca-P that surface of carbon/carbon composite obtains Base biological coating is named as A；
Deposition process conditions are as follows: sedimentation time is 1.0-2.0h, and deposition voltage is 5.0-10.0V, and depositing temperature is 60-80 DEG C, Pulse switching time ratio is 0.25-1.00；
The concentration of the four water-calcium nitrate solution is 1.67 × 10-2-1.67mol/L；
The concentration of the ammonium dihydrogen phosphate is 1.00 × 10-2-1.00mol/L；
Step 2: pulse electrodeposition processing will be carried out after A drying, realizes and introduce catalyst iron in Ca-P base biological coating, name For B；Pulse electrodeposition processing；
Pulse electrodeposition treatment process condition are as follows: six aqueous ferrous sulfate solution concentration of electrolyte is 0.02-2.00g/ml, when deposition Between 0.5-1.5h, deposition voltage be 5.0-10.0V, depositing temperature be 60-80 DEG C, pulse switching time ratio be 0.25-1.00；
Step 3: B is intracavitary as chemical vapor deposition tube furnace, using double injection method deposition of carbon nanotubes, realize in Ca-P Carbon nanotube is evenly dispersed in base biological coating；
The technique of deposition of carbon nanotubes are as follows: at 500 DEG C after hydrogen reducing catalyst iron, at 850 DEG C, argon gas, hydrogen flowing quantity divide Wei not be under the conditions of 400 and 200sccm, using dimethylbenzene as carbon source, ethylenediamine is growth regulator, and injection rate ratio is 7.5, injection time For 1h.
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