CN102644078A - 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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- CN102644078A CN102644078A CN2012101520076A CN201210152007A CN102644078A CN 102644078 A CN102644078 A CN 102644078A CN 2012101520076 A CN2012101520076 A CN 2012101520076A CN 201210152007 A CN201210152007 A CN 201210152007A CN 102644078 A CN102644078 A CN 102644078A
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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; The technology of preparing that relates to the medical implant surface bioactive coating of a kind of tantalum base; The differential arc oxidation of especially a kind of porous tantalic acid calcium and nanometer fibrous Win 40350 double-layer structure coating and hydrothermal preparation technology have the human body hard tissue reparation of good mechanics and biology performance and replace device with structure.
Background technology
Tantalum has excellent biological compatibility, at artificial bone, hip or aspects such as knee joint head prosthesis, plastic sugery the important application potentiality is arranged.But tantalum belongs to bio-inert material, implant in early days can not with the bone forming Chemical bond, do not promote new osteoplastic ability yet, healing time is longer, therefore needs carry out the surface biological activation modification to it.Win 40350 (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 Win 40350 has considerable influence to the bone forming ability.Know that ground substance of bone mainly is made up of with the HA that grows in around it collegen filament, becomes the nanofiber form, cell is unique bone-forming effect to this structure configuration.Even bio-inert material, the adhesion amount of cell on the nanofiber network basal plane of implantation material surface also are higher than the fine and close basal plane of collagen not only far above the fine and close basal plane of homogeneity.The nano shape surface more helps the adhesion and the growth of cell than the micron form.Technology such as existing plasma spraying, laser melting coating, ion beam enhanced depositing, magnetron sputtering, differential arc oxidation can obtain Win 40350 at the compact metal matrix surface; But the Win 40350 that obtains not is nanometer fibrous; Far apart with the crystal habit of inorganic mineral phosphatic rock in the bone, cause it to promote that new osteoplastic ability is lower.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art; The preparation technology of a kind of porous tantalic acid calcium/nanometer fibrous hydroxyapatite bioactive coating is provided; This technology at first adopts differential arc oxidation to prepare the tantalic acid calcium base complex phase layer of calcic and phosphorus at the tantalum matrix surface; Promptly be that the aqueous solution with calcic and phosphorus is electrolytic solution; Adopt the pulse power under high-voltage, the tantalum matrix to be carried out differential arc oxidation, the tantalic acid calcium base complex phase layer to calcic and phosphorus carries out hydrothermal treatment consists under specific thermal and hydric environment condition then.The double-layer structure coating that obtains has following structure and performance characteristic: internal layer (adjoining with matrix) is a tantalic acid calcium base complex phase layer, and promptly a tantalum pentoxide and the tantalum oxide by tantalic acid calcium and trace constitutes, and on form, is multi-cellular structure; The top layer is nanometer fibrous Win 40350, and fiber is to tilt or is parallel to two kinds of orientation of tantalic acid calcium base complex phase layer.Do not have non-continuous face between this double-layer structure coating and the matrix, have high bonding strength.In the pseudo body fluid environment, can form osteolith by rapid induction, have good biological activity.
The objective of the invention is to solve through following technical scheme:
The preparation technology of the double-deck bioactive coating of this tantalum primary surface may further comprise the steps:
1) differential arc oxidation of tantalum:
(CH with 0.1～0.5M
3COO)
2β-C of Ca solution and 0.01～0.06M
3H
7Na
2O
6(β-GP) a kind of or its composite aqueous solution of solution is processed electrolytic solution to P, is that anode, stainless steel are that negative electrode places electrolytic solution with the metal tantalum piece; 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 spacings, 10～40 ℃ of electrolyte temperatures; Differential arc oxidation to tantalum piece carried out 3～20 minutes is handled, and obtains 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:
With concentration is β-C of 0.002～0.04M
3H
7Na
2O
6P solution injects hydrothermal reaction kettle; The solution compactedness is 5%～30%; And tantalic acid calcium base complex phase layer/tantalum piece sample hung on solution top or be soaked in the solution, under 100～200 ℃ condition,, can obtain said double-layer structure coating at tantalum surface to its hydrothermal treatment consists 1～24 hour.
The double-layer structure coating that above method obtains; Internal layer (adjoining with matrix) is a tantalic acid calcium base complex phase layer, and promptly a tantalum pentoxide and the tantalum oxide by tantalic acid calcium and trace constitutes, and its thickness is 24～27 microns; On form, be multi-cellular structure, the aperture is 3～5 microns; The top layer is nanometer fibrous Win 40350, 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.Do not have non-continuous face between this double-layer structure coating and the matrix, have high bonding strength.
The present invention has following beneficial effect:
1) the differential arc oxidation electrolytic solution and the hydrothermal solution composition of the present invention's preparation are simple, are easy to control, do not contain to be prone to decompose composition, and process stabilizing;
2) do not have non-continuous face between double-layer structure coating of the present invention and the matrix, have high bonding strength;
3) bioactive coating that makes of the present invention has good biological activity, in simulated body fluid, can induce Win 40350 fast;
4) the nanofiber form of Win 40350 can significantly promote the adhesion and the growth of cell in the double-layer structure coating of the present invention.
Description of drawings
Fig. 1 uses the present invention to handle the 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 done and to describe in further detail:
Embodiment 1
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled; Obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, its surface and section microscopic appearance SEM photo are consulted Fig. 1 (a) and (b) respectively.The tantalic acid calcium base complex phase layer/tantalum piece sample that obtains after then differential arc oxidation being handled hangs on that concentration is β-C of 0.01M in the hydrothermal reaction kettle
3H
7Na
2O
6The top of the P aqueous solution; The solution compactedness is 15%; Under 140 ℃ of conditions, to its hydrothermal treatment consists 3 hours, can obtain arranging closely, favouring 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 Fig. 2 (a) and (b) respectively.Coating and tantalum high base strength are 36.85N.In the simulated body fluid environment, have good biological activity, the phosphatic rock that induces in the time of 4 days covers the fiber coat surface fully.
Embodiment 2
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled, and obtains the tantalic acid calcium base complex phase layer of calcic and phosphorus.The tantalic acid calcium base complex phase layer/tantalum piece sample that obtains after then differential arc oxidation being handled hangs on that concentration is β-C of 0.01M in the hydrothermal reaction kettle
3H
7Na
2O
6The top of the P aqueous solution; The solution compactedness is 15%, under 140 ℃ condition, to its hydrothermal treatment consists 24 hours, can obtain arranging closely, being 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 Fig. 3 (a) and (b) respectively.Coating and tantalum high base strength are 32N.In the simulated body fluid environment, have good biological activity, the phosphatic rock that induces in the time of 3 days covers the fiber coat surface fully.
Embodiment 3
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled; Obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains after then differential arc oxidation being handled is soaked into that concentration is β-C of 0.01M in the hydrothermal reaction kettle
3H
7Na
2O
6In the P aqueous solution, the solution compactedness is 15%, under 140 ℃ of conditions, to its hydrothermal treatment consists 3 hours, can obtain arranging closely, being 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
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 470 volts of positive voltages, 100 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled; Obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains after then differential arc oxidation being handled is soaked into that concentration is β-C of 0.01M in the hydrothermal reaction kettle
3H
7Na
2O
6In the P aqueous solution, the solution compactedness is 15%, under 140 ℃ of conditions to its hydrothermal treatment consists 24 hours; Can obtain arranging closely, being 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
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 450 volts of positive voltages, 50 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled; Obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, then differential arc oxidation is handled the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains and hang on β-C of 0.002M in the hydrothermal reaction kettle
3H
7Na
2O
6The top of the P aqueous solution, solution compactedness are 15%, under 140 ℃ 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
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 450 volts of positive voltages, 50 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled; Obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains after then differential arc oxidation being handled hangs on β-C of 0.01M in the hydrothermal reaction kettle
3H
7Na
2O
6The top of the P aqueous solution, solution compactedness are 15%, under 140 ℃ 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
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 450 volts of positive voltages, 50 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled; Obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains after then differential arc oxidation being handled hangs on β-C of 0.04M in the hydrothermal reaction kettle
3H
7Na
2O
6The top of the P aqueous solution, solution compactedness are 15%, under 140 ℃ 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
(the CH that will contain 0.2M
3COO)
2β-C of Ca and 0.02M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, stainless steel are negative electrode; Adopt direct current pulse power source; The differential arc oxidation that under the condition of 510 volts of positive voltages, 70 volts of negative voltages, 100 hertz of frequencies, dutycycle 26%, tantalum piece was carried out 5 minutes is handled; Obtain the tantalic acid calcium base complex phase layer of calcic and phosphorus, the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains after then differential arc oxidation being handled hangs on β-C of 0.01M in the hydrothermal reaction kettle
3H
7Na
2O
6The top of the P aqueous solution, solution compactedness are 15%, under 140 ℃ of conditions, to its hydrothermal treatment consists 24 hours, can obtain arranging closely, favouring 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 because overtension, tantalic acid calcium base complex phase laminar surface is except that fiber, and very major part is covered by particulate material.
Embodiment 9
1) differential arc oxidation of the tantalum: (CH that will contain 0.1M
3COO)
2β-C of Ca and 0.01M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, metal stainless steel are that negative electrode places electrolytic solution; 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 spacings, 10 ℃ of electrolyte temperatures; Differential arc oxidation to tantalum piece carried out 3 minutes is handled, and obtains 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: with concentration is β-C of 0.002M
3H
7Na
2O
6The P aqueous solution injects hydrothermal reaction kettle, and the solution compactedness is 5%, and the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains is hung on the solution top, under 100 ℃ of conditions, to its hydrothermal treatment consists 1 hour, can obtain said double-layer structure coating on the tantalum piece surface.
Embodiment 10
1) differential arc oxidation of the tantalum: (CH that will contain 0.5M
3COO)
2β-C of Ca and 0.06M
3H
7Na
2O
6The aqueous solution of P is as electrolytic solution.With the metal tantalum piece is that anode, metal stainless steel are that negative electrode places electrolytic solution; 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 spacings, 40 ℃ of electrolyte temperatures; Differential arc oxidation to tantalum piece carried out 20 minutes is handled, and obtains 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: with concentration is β-C of 0.04M
3H
7Na
2O
6The P aqueous solution injects hydrothermal reaction kettle, and the solution compactedness is 30%, and the tantalic acid calcium base complex phase layer/tantalum piece sample that obtains is soaked in the solution, under 200 ℃ of conditions, to its hydrothermal treatment consists 24 hours, can obtain said double-layer structure coating on the tantalum piece surface.
Embodiment can give an example many; As space is limited, do not list one by one here, in a word; In scope provided by the invention, the bioactive coating that the technology of utilizing differential arc oxidation and hydrothermal treatment consists to combine can obtain having good biological activity and bonding strength at the tantalum matrix surface.
Adopting between double-layer structure coating that preparation technology of the present invention makes and the matrix does not have non-continuous face, has high bonding strength.In the pseudo body fluid environment, can form osteolith by rapid induction, have good biological activity.The top layer of double-layer structure coating is the hydroxyapatite fiber of nano shape, can significantly promote the adhesion and the growth of cell.
Claims (2)
1. the preparation technology of porous tantalic acid calcium/nanometer fibrous hydroxyapatite bioactive coating is characterized in that, may further comprise the steps:
1) differential arc oxidation of tantalum:
(CH with 0.1～0.5M
3COO)
2β-C of Ca solution and 0.01～0.06M
3H
7Na
2O
6(β-GP) a kind of or its composite aqueous solution of solution is processed electrolytic solution to P, is that anode, stainless steel are that negative electrode places electrolytic solution with the metal tantalum piece; 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 spacings, 10～40 ℃ of electrolyte temperatures; Differential arc oxidation to tantalum piece carried out 3～20 minutes is handled, and obtains 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:
With concentration is β-C of 0.002～0.04M
3H
7Na
2O
6P solution injects hydrothermal reaction kettle; The solution compactedness is 5%～30%; And tantalic acid calcium base complex phase layer or tantalum piece sample hung on the solution top or be soaked in the solution, under 100～200 ℃ condition,, promptly obtain coating at tantalum surface to its hydrothermal treatment consists 1～24 hour.
2. based on the described differential arc oxidation of claim 1 and hydrothermal treatment consists combination process double-layer structure coating in the preparation of tantalum matrix surface; It is characterized in that: internal layer is a tantalic acid calcium base complex phase layer; Promptly a tantalum pentoxide and the tantalum oxide by tantalic acid calcium and trace constitutes; Its thickness is 24～27 microns, on form, is multi-cellular structure, and the aperture is 3～5 microns; The 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107998445A (en) * | 2017-12-06 | 2018-05-08 | 吕莉 | A kind of surface modification porous tantalum biomaterial and preparation method thereof |
| CN108042846A (en) * | 2018-01-15 | 2018-05-18 | 陕西科技大学 | A kind of preparation method of strontium doping tantalum pentoxide nanorod structure bioactivity coatings |
| CN113289057A (en) * | 2021-05-19 | 2021-08-24 | 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 |
-
2012
- 2012-05-16 CN CN201210152007.6A patent/CN102644078B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 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》 * |
| HO-JUN SONG,ET AL.: "Fabrication of hydroxyapatite and TiO2 nanorods on microarc-oxidized titanium surface using hydrothermal treatmet", 《APPLIED SURFACE SCIENCE》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107998445A (en) * | 2017-12-06 | 2018-05-08 | 吕莉 | A kind of surface modification porous tantalum biomaterial and preparation method thereof |
| CN108042846A (en) * | 2018-01-15 | 2018-05-18 | 陕西科技大学 | A kind of preparation method of strontium doping tantalum pentoxide nanorod structure bioactivity coatings |
| CN113289057A (en) * | 2021-05-19 | 2021-08-24 | 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 |
| 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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