CN102644078B - Preparation technology of porous calcium gluconate tantalite/nono-funicular hydroxylapatite bioactive coating - Google Patents
Preparation technology of porous calcium gluconate tantalite/nono-funicular hydroxylapatite bioactive coating Download PDFInfo
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- CN102644078B CN102644078B CN201210152007.6A CN201210152007A CN102644078B CN 102644078 B CN102644078 B CN 102644078B CN 201210152007 A CN201210152007 A CN 201210152007A CN 102644078 B CN102644078 B CN 102644078B
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Abstract
The invention discloses a preparation technology of porous calcium gluconate tantalite/nono-funicular hydroxylapatite bioactive coating. The preparation technology comprises the following step of firstly preparing calcium and phosphorus-containing gluconate tantalite-based complex phase layer on the surface of tantalite by a micro arc oxidation technology, i.e. taking calcium and phosphorus-containing water solution as electrolyte, carrying out the micro arc oxidation treatment on the tantalum under high voltage by using a pulse power source, and carrying out the hydro-thermal treatment on the calcium and phosphorus-containing gluconate tantalite-based complex phase layer under a special hydro-thermal environment condition. The obtained coating with a double-layer structure has the following structure and performance characteristics: an inner layer (which is adjacent to a base body) is a gluconate tantalite-based complex phase layer which consists of gluconate tantalite, and a trace amount of antalum pentoxide and tantalum monoxide and is of a microporous structure in shape; and a surface layer is nono-funicular hydroxylapatite, which is inclined to or in parallel with the gluconate tantalite-based complex phase layer. No incontinuous interface exists between the coating with the double-layer structure and the base body, so that the coating is high in combining strength, and the osteolith can be quickly formed in the pseudo body fluid environment in an inducing way, so that the coating is good in biological activity.
Description
Technical field
The invention belongs to medical metal surface biological activation modification technical field, relate to the technology of preparing of the medical implant surface bioactive coating of a kind of tantalum base, especially the differential arc oxidation of porous tantalic acid calcium and nanometer fibrous hydroxyapatite double-layer structure coating and a hydro-thermal technology of preparing, to build the human body hard tissue reparation and replacement device with good mechanics and biology performance.
Background technology
Tantalum has good biocompatibility, has important application potentiality at aspects such as artificial bone, hip or knee joint head prosthesis, plastic surgeries.But tantalum belongs to bio-inert material, implant in early days can not with bone forming Chemical bond, do not promote new osteoplastic ability yet, healing time is longer, therefore needs it to carry out surface biological activation modification.Hydroxyapatite (HA) is the important component of skeleton, possesses good biological activity, promotes that new osteoplastic ability is higher, is the good selection of carrying out material surface modifying.The form of hydroxyapatite has considerable influence to bone forming ability.Know, ground substance of bone is mainly made up of with the HA growing in around it collegen filament, becomes nanofiber form, and cell is unique bone-forming effect to this structural configuration.Even bio-inert material, the adhesion amount of cell on the nanofiber network basal plane of implantation material surface is not only far above the fine and close basal plane of homogeneity, also higher than the fine and close basal plane of collagen.Nano shape surface is more conducive to adhesion and the growth of cell than micron form.The technology such as existing plasma spraying, laser melting coating, ion beam enhanced depositing, magnetron sputtering, differential arc oxidation can obtain hydroxyapatite at compact metal matrix surface, but the hydroxyapatite obtaining not is nanometer fibrous, far apart with the crystal habit of inorganic mineral phosphatic rock in bone, cause it to promote that new osteoplastic ability is lower.
Summary of the invention
The object of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of preparation technology of porous tantalic acid calcium/nanometer fibrous hydroxyapatite bioactive coating is provided, first this technique adopt differential arc oxidation to prepare the tantalic acid calcium base complex phase layer of calcic and phosphorus at tantalum matrix surface, be that the aqueous solution taking calcic and phosphorus is as electrolytic solution, adopt the pulse power, under high-voltage, tantalum matrix is carried out to differential arc oxidation, then under specific thermal and hydric environment condition, the tantalic acid calcium base complex phase layer of calcic and phosphorus is carried out to hydrothermal treatment consists.The double-layer structure coating obtaining has following structure and performance characteristic: internal layer (adjoining with matrix) is tantalic acid calcium base complex phase layer, is made up of tantalum pentoxide and a tantalum oxide of tantalic acid calcium and trace, is multi-cellular structure in form; Top layer is nanometer fibrous hydroxyapatite, and fiber is to tilt or is parallel to two kinds of orientation of tantalic acid calcium base complex phase layer.Between this double-layer structure coating and matrix, without non-continuous face, there is high bonding strength.In pseudo body fluid environment, can form osteolith by rapid induction, there is good biological activity.
The object of the invention is to solve by the following technical programs:
The preparation technology of the double-deck bioactive coating of this tantalum primary surface, comprises the following steps:
1) differential arc oxidation of tantalum:
By (the CH of 0.1～0.5M
3cOO)
2β-C of Ca solution and 0.01～0.06M
3h
7na
2o
6p(β-GP) one or its composite aqueous solution of solution makes electrolytic solution, taking metal tantalum piece as anode, stainless steel is placed in electrolytic solution as negative electrode; Adopt direct current pulse power source, under the condition of 450～510 volts of positive voltages, 50～100 volts of negative voltages, 50～3000 hertz of frequencies, dutycycle 10～40%, 8～10 centimetres of cathode-anode plate spacing, 10～40 DEG C of electrolyte temperatures, tantalum piece is carried out to the differential arc oxidation processing of 3～20 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus;
2) hydrothermal treatment consists of the tantalic acid calcium base complex phase layer of calcic and phosphorus:
β-the C that is 0.002～0.04M by concentration
3h
7na
2o
6p solution injects hydrothermal reaction kettle, solution compactedness is 5%～30%, and tantalic acid calcium base complex phase layer/tantalum piece sample is hung on to solution top or is soaked in solution, under the condition of 100～200 DEG C, to its hydrothermal treatment consists 1～24 hour, can obtain described double-layer structure coating at tantalum surface.
The double-layer structure coating that above method obtains, internal layer (adjoining with matrix) is tantalic acid calcium base complex phase layer, is made up of tantalum pentoxide and a tantalum oxide of tantalic acid calcium and trace, and its thickness is 24～27 microns, in form, be multi-cellular structure, aperture is 3～5 microns; Top layer is nanometer fibrous hydroxyapatite, and Fibre diameter is 40～90 nanometers, is to tilt or is parallel to two kinds of orientation of tantalic acid calcium base complex phase layer.Between this double-layer structure coating and matrix, without non-continuous face, there is high bonding strength.
The present invention has following beneficial effect:
1) differential arc oxidation electrolytic solution and the hydrothermal solution composition of the present invention's preparation are simple, are easy to control, not containing easily decomposing composition and process stabilizing;
2) between double-layer structure coating of the present invention and matrix without non-continuous face, there is high bonding strength;
3) bioactive coating that the present invention makes has good biological activity, in simulated body fluid, can induce fast hydroxyapatite;
4) in double-layer structure coating of the present invention, the nanofiber form of hydroxyapatite can significantly promote adhesion and the growth of cell.
Brief description of the drawings
Fig. 1 uses the present invention to process surface topography and the cross-section morphology SEM photo of the tantalic acid calcium base complex phase layer (embodiment 1 differential arc oxidation layer) of prepared phosphorous and calcium through differential arc oxidation;
Fig. 2 uses surface topography and the cross-section morphology SEM photo of the present invention through differential arc oxidation and the prepared fiber coat of hydrothermal treatment consists recombining process (embodiment 1 coating);
Fig. 3 uses surface topography and the cross-section morphology SEM photo of the present invention through differential arc oxidation and the prepared fiber coat of hydrothermal treatment consists recombining process (embodiment 2 coatings);
Fig. 4 uses the surface topography SEM photo of the present invention through differential arc oxidation and the prepared fiber coat of hydrothermal treatment consists recombining process (embodiment 4 coatings).
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail:
Embodiment 1
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, its surface and section microscopic appearance SEM photo are consulted respectively Fig. 1 (a) and (b).Then the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining after differential arc oxidation being processed hangs on β-C that in hydrothermal reaction kettle, concentration is 0.01M
3h
7na
2o
6the top of the P aqueous solution, solution compactedness is 15%, under 140 DEG C of conditions to its hydrothermal treatment consists 3 hours, can obtain arranging closely, favour the fiber of tantalic acid calcium base complex phase layer, Fibre diameter is 40～60 nanometers, length is 0.3～0.5 micron, and its surface and section microscopic appearance SEM photo are consulted respectively Fig. 2 (a) and (b).The bonding strength of coating and tantalum matrix is 36.85N.In simulated body fluid environment, have good biological activity, the phosphatic rock inducing 4 days time covers fiber coat surface completely.
Embodiment 2
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus.Then the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining after differential arc oxidation being processed hangs on β-C that in hydrothermal reaction kettle, concentration is 0.01M
3h
7na
2o
6the top of the P aqueous solution, solution compactedness is 15%, under the condition of 140 DEG C to its hydrothermal treatment consists 24 hours, can obtain arranging closely, be parallel to the fiber of tantalic acid calcium base complex phase layer, Fibre diameter is about 40～60 nanometers, length is greater than 3 microns, and fibrolaminar thickness is about 1 micron, and its surface and section microscopic appearance SEM photo are consulted respectively Fig. 3 (a) and (b).The bonding strength of coating and tantalum matrix is 32N.In simulated body fluid environment, have good biological activity, the phosphatic rock inducing 3 days time covers fiber coat surface completely.
Embodiment 3
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining after then differential arc oxidation being processed is soaked into β-C that in hydrothermal reaction kettle, concentration is 0.01M
3h
7na
2o
6in the P aqueous solution, solution compactedness is 15%, under 140 DEG C of conditions, to its hydrothermal treatment consists 3 hours, can obtain arranging closely, be parallel to the fiber of tantalic acid calcium base complex phase layer, and Fibre diameter is about 40～60 nanometers, and length is about 1 micron.
Embodiment 4
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining after then differential arc oxidation being processed is soaked into β-C that in hydrothermal reaction kettle, concentration is 0.01M
3h
7na
2o
6in the P aqueous solution, solution compactedness is 15%, under 140 DEG C of conditions to its hydrothermal treatment consists 24 hours, can obtain arranging closely, be parallel to the fiber of tantalic acid calcium base complex phase layer, Fibre diameter is about 40～60 nanometers, and length is greater than 3 microns, and its surface microscopic topographic SEM photo is consulted Fig. 4.
Embodiment 5
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 450 volts of positive voltages, 50 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample then differential arc oxidation processing being obtained hangs on the β-C of 0.002M in hydrothermal reaction kettle
3h
7na
2o
6the top of the P aqueous solution, solution compactedness is 15%, under 140 DEG C of conditions, to its hydrothermal treatment consists 24 hours, can obtain fiber sparse, that be parallel to tantalic acid calcium base complex phase layer, and Fibre diameter is about 40 nanometers, and length is about 300 nanometers.
Embodiment 6
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 450 volts of positive voltages, 50 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining after then differential arc oxidation being processed hangs on the β-C of 0.01M in hydrothermal reaction kettle
3h
7na
2o
6the top of the P aqueous solution, solution compactedness is 15%, under 140 DEG C of conditions, to its hydrothermal treatment consists 24 hours, can obtain fiber sparse, that be parallel to tantalic acid calcium base complex phase layer, and Fibre diameter is about 40 nanometers, and length is about 1 micron.
Embodiment 7
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 450 volts of positive voltages, 50 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining after then differential arc oxidation being processed hangs on the β-C of 0.04M in hydrothermal reaction kettle
3h
7na
2o
6the top of the P aqueous solution, solution compactedness is 15%, under 140 DEG C of conditions, to its hydrothermal treatment consists 24 hours, can obtain fiber sparse, that be parallel to tantalic acid calcium base complex phase layer, and Fibre diameter is about 90 nanometers, and length is greater than 2 microns.
Embodiment 8
By (the CH containing 0.2M
3cOO)
2β-C of Ca and 0.02M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, stainless steel is negative electrode, adopt direct current pulse power source, under the condition of 510 volts of positive voltages, 70 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece is carried out to the differential arc oxidation processing of 5 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining after then differential arc oxidation being processed hangs on the β-C of 0.01M in hydrothermal reaction kettle
3h
7na
2o
6the top of the P aqueous solution, solution compactedness is 15%, under 140 DEG C of conditions, to its hydrothermal treatment consists 24 hours, can obtain arranging closely, favour the fiber of tantalic acid calcium base complex phase layer, and Fibre diameter is about 40～60 nanometers, and length is about 1 micron.But due to overtension, tantalic acid calcium base complex phase layer surface, except fiber, very most ofly covered by particulate material.
Embodiment 9
1) differential arc oxidation of tantalum the: by (CH containing 0.1M
3cOO)
2β-C of Ca and 0.01M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, metal stainless steel is placed in electrolytic solution as negative electrode; Adopt direct current pulse power source, under the condition of 450 volts of positive voltages, 50 volts of negative voltages, 50 hertz of frequencies, dutycycle 10%, 8 centimetres of cathode-anode plate spacing, 10 DEG C of electrolyte temperatures, tantalum piece is carried out to the differential arc oxidation processing of 3 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus.
2) hydrothermal treatment consists of the tantalic acid calcium base complex phase layer of calcic and phosphorus: the β-C that is 0.002M by concentration
3h
7na
2o
6the P aqueous solution injects hydrothermal reaction kettle, and solution compactedness is 5%, and the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining is hung on to solution top, under 100 DEG C of conditions, to its hydrothermal treatment consists 1 hour, can obtain on tantalum piece surface described double-layer structure coating.
Embodiment 10
1) differential arc oxidation of tantalum the: by (CH containing 0.5M
3cOO)
2β-C of Ca and 0.06M
3h
7na
2o
6the aqueous solution of P is as electrolytic solution.Taking metal tantalum piece as anode, metal stainless steel is placed in electrolytic solution as negative electrode; Adopt direct current pulse power source, under the condition of 510 volts of positive voltages, 100 volts of negative voltages, 3000 hertz of frequencies, dutycycle 40%, 10 centimetres of cathode-anode plate spacing, 40 DEG C of electrolyte temperatures, tantalum piece is carried out to the differential arc oxidation processing of 20 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus;
2) hydrothermal treatment consists of the tantalic acid calcium base complex phase layer of calcic and phosphorus: the β-C that is 0.04M by concentration
3h
7na
2o
6the P aqueous solution injects hydrothermal reaction kettle, and solution compactedness is 30%, and the tantalic acid calcium base complex phase layer/tantalum piece sample obtaining is soaked in solution, under 200 DEG C of conditions, to its hydrothermal treatment consists 24 hours, can obtain on tantalum piece surface described double-layer structure coating.
Embodiment can exemplify many, as space is limited, do not list one by one here, in a word, in scope provided by the invention, utilize technology that differential arc oxidation and hydrothermal treatment consists combine can obtain having at tantalum matrix surface the bioactive coating of good biological activity and bonding strength.
Adopt between double-layer structure coating that preparation technology of the present invention makes and matrix without non-continuous face, there is high bonding strength.In pseudo body fluid environment, can form osteolith by rapid induction, there is good biological activity.The top layer of double-layer structure coating is the hydroxyapatite fiber of nano shape, can significantly promote adhesion and the growth of cell.
Claims (2)
1. a preparation technology for porous tantalic acid calcium/nanometer fibrous hydroxyapatite bioactive coating, is characterized in that, comprises the following steps:
1) differential arc oxidation of tantalum:
By (the CH of 0.1～0.5M
3cOO)
2β-C of Ca solution and 0.01～0.06M
3h
7na
2o
6the composite aqueous solution of P solution is made electrolytic solution, taking metal tantalum piece as anode, stainless steel is placed in electrolytic solution as negative electrode; Adopt direct current pulse power source, under the condition of 450～510 volts of positive voltages, 50～100 volts of negative voltages, 50～3000 hertz of frequencies, dutycycle 10～40%, 8～10 centimetres of cathode-anode plate spacing, 10～40 DEG C of electrolyte temperatures, tantalum piece is carried out to the differential arc oxidation processing of 3～20 minutes, obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus;
2) hydrothermal treatment consists of the tantalic acid calcium base complex phase layer of calcic and phosphorus:
β-the C that is 0.002～0.04M by concentration
3h
7na
2o
6p solution injects hydrothermal reaction kettle, and solution compactedness is 5%～30%, and tantalic acid calcium base complex phase layer sample hung on to solution top or be soaked in solution, under the condition of 100～200 DEG C, to its hydrothermal treatment consists 1～24 hour, obtains coating at tantalum surface.
2. the double-layer structure coating that preparation technology according to claim 1 is prepared at tantalum matrix surface, it is characterized in that: internal layer is tantalic acid calcium base complex phase layer, formed by tantalum pentoxide and a tantalum oxide of tantalic acid calcium and trace, its thickness is 24～27 microns, in form, be multi-cellular structure, aperture is 3～5 microns; Top layer is nanometer fibrous hydroxyapatite, and Fibre diameter is 40～90 nanometers, is to tilt or is parallel to two kinds of orientation of tantalic acid calcium base complex phase layer.
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| CN201210152007.6A CN102644078B (en) | 2012-05-16 | 2012-05-16 | Preparation technology of porous calcium gluconate tantalite/nono-funicular hydroxylapatite bioactive coating |
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| CN107998445A (en) * | 2017-12-06 | 2018-05-08 | 吕莉 | A kind of surface modification porous tantalum biomaterial and preparation method thereof |
| CN108042846B (en) * | 2018-01-15 | 2020-11-24 | 陕西科技大学 | Preparation method of strontium-doped tantalum oxide nanorod structure bioactive coating |
| CN113289057B (en) * | 2021-05-19 | 2022-10-14 | 北京爱康宜诚医疗器材有限公司 | Tantalum-coated orthopedic implant material, preparation method thereof and orthopedic implant |
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Non-Patent Citations (5)
| Title |
|---|
| Coatings Technology》.2010,第204卷第2273-2278. * |
| Fabrication of hydroxyapatite and TiO2 nanorods on microarc-oxidized titanium surface using hydrothermal treatmet;Ho-Jun Song,et al.;《Applied Surface Science》;20100524;第256卷;第7056-7061页 * |
| Ho-Jun Song，et al..Effect of the electric conditions of AC-type microarc oxidation and hydrothermal treatment solution on the characteristics of hydroxyapatite formed on titanium.《Surface & Coatings Technology》.2010,第204卷第2273-2278. |
| Ho-Jun Song,et al..Effect of the electric conditions of AC-type microarc oxidation and hydrothermal treatment solution on the characteristics of hydroxyapatite formed on titanium.《Surface & * |
| Ho-Jun Song,et al..Fabrication of hydroxyapatite and TiO2 nanorods on microarc-oxidized titanium surface using hydrothermal treatmet.《Applied Surface Science》.2010,第256卷第7056-7061页. |
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