CN109722660A - A kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings and preparation method thereof - Google Patents
A kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings and preparation method thereof Download PDFInfo
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- CN109722660A CN109722660A CN201811627397.1A CN201811627397A CN109722660A CN 109722660 A CN109722660 A CN 109722660A CN 201811627397 A CN201811627397 A CN 201811627397A CN 109722660 A CN109722660 A CN 109722660A
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Abstract
The invention discloses a kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings and preparation method thereof, first using the aqueous solution of hydrofluoric acid containing and hydrogen peroxide as hydrothermal solution, hydro-thermal process is carried out to tantalum matrix using different hydrothermal conditions, then hydro-thermal process is carried out to the tantalum oxide nanorod structure coating of acquisition again under the conditions of the thermal and hydric environment of calcic, obtained coating microstrueture is in nano bar-shape, object is mutually tantalum pentoxide, doped with calcium constituent in nanorod structure coating, there is high bond strength between the calcium analysis nanorod structure coating and matrix, calcium constituent is from the precipitation in coating as the extension of soaking time gradually increases, energy rapid induction forms osteolith in pseudo body fluid environment, with good bioactivity.
Description
Technical field
The invention belongs to medical metal surface biological activation modification technical fields, are related to a kind of tantalum base medical implant surface
The technology of preparing of bioactivity coatings, and in particular to a kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings and its preparation
Method.
Background technique
Compared with the hard tissue implanting materials such as existing titanium or titanium alloy, zirconium, magnesium alloy, the excellent corrosion resistance of tantalum and biology
Compatibility makes it have broad application prospects in the fields such as bone substitute and Dental implantion.Low elastic modulus, Gao Rong in recent years
The development of the porous tantalum of product porosity and great friction coefficient makes tantalum in spinal interbody fusion, hip or knee replacements, treatment stock
Head necrosis etc. has even more important application potential.But tantalum does not have bioactivity as a kind of inert metal, plants
It is difficult to form synostosis with bone tissue after entering human body, it is therefore desirable to longer treatment time.It is excellent in order to obtain bioactivity
Tantalum implant, it is modified bioactivation need to be carried out to its surface.Studies have shown that implant material surface nanoscale structure feature
There is important influence especially to osteogenesis functions such as the adherency of osteoblast, proliferation and mineralisings cell behavior, has obvious
Regulating and controlling effect effect, then have an immense impact on to the bone fusion of implant material and host bone tissue.Meanwhile Ca2+It is people
The one of the chief elements of body bone, calcium ion is introduced into surface modified coat can be by promoting implant surfaces osteoblast
Proliferation is to reduce human body to the rejection of implant.Ta2O5There is significant contribution to the corrosion resistance of tantalum metal surface, but thinks
Ta is prepared in tantalum surface2O5Nano structure coating has the methods of anodic oxidation, magnetron sputtering, but anode oxidation method exists
The problem of conjugation difference, magnetically controlled sputter method belong to linear technique between coating and matrix, are not easy portion's realization in the porous material
Coating preparation.In view of the above problems, the high oxidation of bond strength can be prepared in porous tantalum surface and inside by expecting to have one kind
The method of tantalum nano-structure bioactive coating.
Summary of the invention
The purpose of the present invention is to provide a kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings and its preparation sides
Method is tied between nano-structure bioactive coating and matrix prepared by the present invention with overcoming the problems of the above-mentioned prior art
It closes closely, there is high bond strength and good bioactivity, apatite can be quickly induced in simulated body fluid environment,
To construct there is the human body hard tissue of good mechanics and biology performance to be implanted into material.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings, comprising the following steps:
Step 1: it prepares and contains HF and H2O2Aqueous solution be soaked into hydrothermal solution as hydrothermal solution, and by tantalum sample
In, hydro-thermal process is carried out to it, obtains tantalum oxide nanorod structure coating in tantalum primary surface to get to treated tantalum sample;
Step 2: calcium acetate is configured to containing calcium solution, and will treated that tantalum sample is soaked into containing in calcium solution, to it
Hydro-thermal process is carried out, i.e., obtains calcium analysis tantalum oxide nanorod structure bioactivity coatings in tantalum surface.
Further, the concentration of HF is 0.2~0.4mol/L, H in step 1 hydrothermal solution2O2The concentration of solution be 1~
2mol/L。
Further, hydrothermal solution is injected in hydrothermal reaction kettle in step 1, makes solution compactedness 40%~60%,
Then tantalum sample is soaked into hydrothermal solution and carries out hydro-thermal process.
Further, the temperature of hydro-thermal process is 220~240 DEG C in step 1, and the time is 12~24 hours.
Further, the concentration in step 2 containing calcium solution is 0.001~0.1mol/L.
Further, it will contain in step 2 in calcium solution injection hydrothermal reaction kettle, and make solution compactedness 40%~60%,
Then the step 1 tantalum sample that obtains that treated is soaked into hydrothermal solution and carries out hydro-thermal process.
Further, the temperature of hydro-thermal process is 200 DEG C in step 2, and the time is 1~6 hour.
A kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings, microstructure are in upright nano bar-shape, nanometer
Stick diameter is 20~100 nanometers.
Further, the foreign atom percentage of calcium constituent is in calcium analysis tantalum oxide nanorod structure bioactivity coatings
4.15~13.26%.
Further, calcium analysis tantalum oxide nanorod structure bioactivity coatings surface roughness Ra is received for 100~110
Rice.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention uses hydro-thermal process method to prepare tantalum oxide nanorod structure in tantalum matrix surface first, is with hydrogeneous fluorine
The solution of acid and hydrogen peroxide is hydrothermal solution, is carried out at hydro-thermal using different hydrothermal temperatures, hydro-thermal time conditions to tantalum matrix
Then reason carries out hydro-thermal process, hydrothermal solution ingredient to the tantalum oxide nanorod structure coating of above-mentioned acquisition in containing calcium solution
Simply, easily controllable, without easily decomposition ingredient, and process stabilizing.
Further, by control condition, the calcium constituent that is adulterated in nano-structure bioactive coating prepared by the present invention
Precipitation Behavior show rule first quick and back slow, it can be achieved that element be precipitated effective control, and then control its as implantation
Bone-forming effect when body material surface coating.
Further, by control condition, nano-structure bioactive coating prepared by the present invention is in simulated body fluid environment
In there is good bioactivity, coating surface has induced a large amount of osteoliths at 6 days, the apatite that 9 days whens induce
Nanometer rods coating surface is completely covered.
The coating that the present invention obtains has the following structure and performance characteristic: coating microstrueture is in nano bar-shape, the nanometer
The size and stick spacing of stick can significantly promote the adherency and proliferation of cell, and object is mutually tantalum pentoxide, in nanorod structure coating
Doped with calcium constituent, the binding ability between the calcium analysis nanometer rods coating and matrix is preferable, has high bond strength, obtains
Coating Surface Roughness it is smaller, calcium constituent shows rule first quick and back slow from the precipitation in coating, in pseudo body fluid environment
Energy rapid induction forms osteolith, has good bioactivity.
Detailed description of the invention
Fig. 1 is that the calcium tantalum oxide nanorod structure coating surface SEM that mixes prepared by embodiment 3 schemes;
Fig. 2 is that the calcium tantalum oxide nanorod structure coating surface EDS that mixes prepared by embodiment 3 schemes;
Fig. 3 is that calcium tantalum oxide nanorod structure coating of mixing prepared by embodiment 3 impregnates 6 days rear surface shapes in simulated body fluid
The scanning figure of looks.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings, comprising the following steps:
1) hydro-thermal process of tantalum:
With 0.2~0.4mol/L HF and 1~2mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydro-thermal reaction
In kettle, solution compactedness is 40%~60%, and tantalum sample is soaked into solution, to its water under conditions of 220~240 DEG C
Heat treatment 12~24 hours can obtain tantalum oxide nanorod structure coating in tantalum primary surface to get to treated tantalum sample;
2) the secondary hydro-thermal process of tantalum oxide nanorod structure coating:
The calcium acetate solution that concentration is 0.001~0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 40%
~60%, and will treated that tantalum sample is soaked into containing in calcium solution, it is small to its hydro-thermal process 1~6 under conditions of 200 DEG C
When, the calcium analysis tantalum oxide nanorod structure coating can be obtained in tantalum surface.
The coating microstrueture being prepared is in upright nano bar-shape, and object is mutually tantalum pentoxide, nanorod diameter 20
~100 nanometers.Doped with calcium constituent in nanorod structure coating, the foreign atom percentage of calcium constituent is 4.15~13.26%.
There is high bond strength between the calcium analysis nanorod structure coating and matrix.The Coating Surface Roughness of acquisition is smaller, slightly
Rugosity Ra is 100 rans.Calcium constituent shows rule first quick and back slow from the precipitation in coating, soaks in pseudo body fluid environment
Sample surfaces energy rapid induction forms osteolith after bubble 3~9 days, has good bioactivity.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
With 0.2mol/L HF and 1mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 60%, and tantalum sample is soaked into solution, to its hydro-thermal process 24 hours under conditions of 220 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating, and coating microstrueture is in upright nano bar-shape, and nanometer rods average diameter is
28 nanometers, nanorod length is about 100~200 nanometers, and roughness Ra is about 96.3 ± 9.5 nanometers.
The calcium acetate solution that concentration is 0.001mol/L is injected in hydrothermal reaction kettle, solution compactedness is 60%, and will
The tantalum based specimen for being covered with tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its water under conditions of 200 DEG C
Heat treatment 2 hours, can obtain the calcium analysis tantalum oxide nanorod structure coating in tantalum surface.Coating microstrueture is still in
Upright nano bar-shape, object are mutually tantalum pentoxide, doped with calcium constituent, the foreign atom hundred of calcium constituent in nanorod structure coating
Divide than being 4.15%.Nanorod diameter, length and there is no significant change before mixing calcium.
Embodiment 2
With 0.2mol/L HF and 1mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 60%, and tantalum sample is soaked into solution, to its hydro-thermal process 24 hours under conditions of 220 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating, and coating microstrueture is in upright nano bar-shape, and nanometer rods average diameter is
28 nanometers, nanorod length is about 100~200 nanometers, and roughness Ra is about 96.3 ± 9.5 nanometers.
The calcium acetate solution that concentration is 0.01mol/L is injected in hydrothermal reaction kettle, solution compactedness is 60%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 2 hours, can obtain the calcium analysis tantalum oxide nanorod structure coating in tantalum surface.Coating manufactured in the present embodiment is micro-
Seeing structure is in upright nano bar-shape, and object is mutually tantalum pentoxide, nanorod diameter, length and does not have significant change before mixing calcium, is received
Doped with calcium constituent in rice stick structure coating, the foreign atom percentage of calcium constituent is 10.31%.
Embodiment 3
With 0.2mol/L HF and 1mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 60%, and tantalum sample is soaked into solution, to its hydro-thermal process 24 hours under conditions of 220 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating, and coating microstrueture is in upright nano bar-shape, and nanometer rods average diameter is
28 nanometers, nanorod length is about 100~200 nanometers, and roughness Ra is about 96.3 ± 9.5 nanometers.
The calcium acetate solution that concentration is 0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 60%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 2 hours, can obtain the calcium analysis tantalum oxide nanorod structure coating in tantalum surface.Coating microstrueture is still in straight
Vertical nano bar-shape, object are mutually tantalum pentoxide, nanorod diameter, length and do not have significant change, nanometer rods coating table before mixing calcium
Face pattern refering to fig. 1, doped with calcium constituent in nanorod structure coating, EDS picture referring to Fig.2, calcium constituent foreign atom hundred
Divide than being 11.97%.There is good bioactivity in simulated body fluid environment, coating surface has induced largely at 6 days
Osteolith, for surface topography SEM picture refering to Fig. 3, nanometer rods coating surface is completely covered in the apatite that 9 days whens induce.And
The nanorod structure coating for not mixing calcium at this time starts to induce apatite not yet.It is impregnated in 0.9%NaCl normal saline solution,
With the extension of soaking time, the amount of precipitation of calcium ion increases.Roughness Ra is about 100.3 ± 9.1 nanometers.
Embodiment 4
With 0.2mol/L HF and 1mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 60%, and tantalum sample is soaked into solution, to its hydro-thermal process 24 hours under conditions of 220 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating, and coating microstrueture is in upright nano bar-shape, and nanometer rods average diameter is
28 nanometers, nanorod length is about 100~200 nanometers, and roughness Ra is about 96.3 ± 9.5 nanometers.
The calcium acetate solution that concentration is 0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 60%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 1 hour, can obtain the calcium analysis tantalum oxide nanorod structure coating in tantalum surface.Coating microstrueture is in uprightly to receive
Rice is rodlike, and object is mutually tantalum pentoxide, nanorod diameter and changes less before mixing calcium, doped with calcium member in nanorod structure coating
Element, the foreign atom percentage of calcium constituent are 8.20%.
Embodiment 5
With 0.2mol/L HF and 1mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 60%, and tantalum sample is soaked into solution, to its hydro-thermal process 24 hours under conditions of 220 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating, and coating microstrueture is in upright nano bar-shape, and nanometer rods average diameter is
28 nanometers, nanorod length is about 100~200 nanometers, and roughness Ra is about 96.3 ± 9.5 nanometers.
The calcium acetate solution that concentration is 0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 60%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 6 hours, can obtain the calcium analysis tantalum oxide nanorod structure coating in tantalum surface.Coating microstrueture is in uprightly to receive
Rice is rodlike, and object is mutually tantalum pentoxide, nanorod diameter and changes less before mixing calcium, doped with calcium member in nanorod structure coating
Element, the foreign atom percentage of calcium constituent are 13.26%.
Embodiment 6
With 0.2mol/L HF and 1mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 40%, and tantalum sample is soaked into solution, to its hydro-thermal process 24 hours under conditions of 240 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating, and coating microstrueture is in upright nano bar-shape, and nanorod diameter is about 100
Nanometer, nanorod length is about 1 micron.
The calcium acetate solution that concentration is 0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 40%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 2 hours, can obtain calcium analysis tantalum oxide nanorod structure coating in tantalum surface.
Embodiment 7
With 0.4mol/L HF and 2mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 40%, and tantalum sample is soaked into solution, to its hydro-thermal process 24 hours under conditions of 240 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating, and coating microstrueture is in upright nano bar-shape, and nanorod diameter is about 20
Nanometer;
The calcium acetate solution that concentration is 0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 40%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 2 hours, can obtain calcium analysis tantalum oxide nanorod structure coating in tantalum surface.
Embodiment 8
With 0.2mol/L HF and 1mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, solution
Compactedness is 60%, and tantalum sample is soaked into solution, to its hydro-thermal process 12 hours under conditions of 220 DEG C, Ji Ke
Tantalum primary surface obtains tantalum oxide nanorod structure coating;
The calcium acetate solution that concentration is 0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 60%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 2 hours, can obtain calcium analysis tantalum oxide nanorod structure coating in tantalum surface.
Embodiment 9
With 0.3mol/L HF and 1.5mol/L H2O2Molar concentration prepare hydrothermal solution, inject hydrothermal reaction kettle in, it is molten
Liquid compactedness is 50%, and tantalum sample is soaked into solution, to its hydro-thermal process 18 hours under conditions of 230 DEG C
Tantalum oxide nanorod structure coating is obtained in tantalum primary surface;
The calcium acetate solution that concentration is 0.1mol/L is injected in hydrothermal reaction kettle, solution compactedness is 50%, and will be covered
The tantalum based specimen for being stamped tantalum oxide nanorod structure coating is soaked into calcium acetate solution, to its hydro-thermal under conditions of 200 DEG C
Processing 2 hours, can obtain calcium analysis tantalum oxide nanorod structure coating in tantalum surface.
Using non-continuous face is not present between nanorod structure coating and matrix made from preparation process of the invention, have
There is high bond strength.Energy rapid induction forms osteolith in pseudo body fluid environment, has good bioactivity.Tantalum oxide
The nanostructure of coating can significantly promote the adherency and growth of cell, and the calcium constituent adulterated in nanorod structure coating will effectively promote
Into the mineralising of osteoblast.
Claims (10)
1. a kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings, which is characterized in that including following step
It is rapid:
Step 1: it prepares and contains HF and H2O2Aqueous solution be soaked into hydrothermal solution as hydrothermal solution, and by tantalum sample, it is right
It carries out hydro-thermal process, obtains tantalum oxide nanorod structure coating in tantalum primary surface to get to treated tantalum sample;
Step 2: calcium acetate is configured to containing calcium solution, and by treated, tantalum sample is soaked into containing in calcium solution, is carried out to it
Hydro-thermal process obtains calcium analysis tantalum oxide nanorod structure bioactivity coatings in tantalum surface.
2. a kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 1,
It is characterized in that, the concentration of HF is 0.2~0.4mol/L, H in step 1 hydrothermal solution2O2The concentration of solution is 1~2mol/L.
3. a kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 1,
It is characterized in that, hydrothermal solution is injected in hydrothermal reaction kettle in step 1, makes solution compactedness 40%~60%, then by tantalum
Sample, which is soaked into hydrothermal solution, carries out hydro-thermal process.
4. a kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 1,
It is characterized in that, the temperature of hydro-thermal process is 220~240 DEG C in step 1, and the time is 12~24 hours.
5. a kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 1,
It is characterized in that, the concentration in step 2 containing calcium solution is 0.001~0.1mol/L.
6. a kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 1,
It is characterized in that, will contain in calcium solution injection hydrothermal reaction kettle in step 2, and make solution compactedness 40%~60%, it then will step
The rapid one tantalum sample that obtains that treated, which is soaked into hydrothermal solution, carries out hydro-thermal process.
7. a kind of preparation method of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 1,
It is characterized in that, the temperature of hydro-thermal process is 200 DEG C in step 2, and the time is 1~6 hour.
8. a kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings, using the described in any item preparations of claim 1-7
Method is made, which is characterized in that and calcium analysis tantalum oxide nanorod structure bioactivity coatings microstructure is in upright nano bar-shape,
Nanorod diameter is 20~100 nanometers.
9. a kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 8, which is characterized in that calcium
The foreign atom percentage for adulterating calcium constituent in tantalum oxide nanorod structure bioactivity coatings is 4.15~13.26%.
10. a kind of calcium analysis tantalum oxide nanorod structure bioactivity coatings according to claim 8, which is characterized in that
Calcium analysis tantalum oxide nanorod structure bioactivity coatings surface roughness Ra is 100~110 nanometers.
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CN114159626A (en) * | 2021-11-30 | 2022-03-11 | 陕西科技大学 | Sodium tantalate film with bioactivity and antibacterial property and preparation method thereof |
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RU2416434C1 (en) * | 2009-12-24 | 2011-04-20 | Анатолий Алексеевич Кулаков | Bioengineered structure for bony defect closure and osteogenesis and method for producing said structure |
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