CN108295307A - A kind of bone implantation calcium phosphorous compound-magnesium composite coating and preparation method thereof - Google Patents
A kind of bone implantation calcium phosphorous compound-magnesium composite coating and preparation method thereof Download PDFInfo
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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Abstract
In order to solve the synosteosis and infection problems of implantation material, the present invention provides a kind of bone implantation calcium phosphorous compound magnesium composite coatings and preparation method thereof, using using anti-raw sedimentation and evaporation coating technique, hydroxyapatite magnesium metal coating is prepared on titanium or titanium alloy, cobalt-base alloys, stainless steel solid, the thickness of the coating is 6 220 μm.The present invention can promote the compatibility of the implantation material of bone and mouth cavity planting body and help solve infection problems, has splendid biocompatibility by the implantation material prepared by the method, meet the standard requirement of implant site mechanical property, and has effective sterilizing function.
Description
Technical field
The present invention relates to field of medical materials, more particularly to after gear division implantation material, wound orthopaedics fix, joint replacement and people
The packing material of body tissue defect and implantation material antimicrobial technology field, more particularly to a kind of bone implantation calcium phosphorous compound-
Magnesium composite coating and preparation method thereof
Background technology
Since the undesirable cell reaction that implantation prosthetic loosening and abrasion cause makes the implants such as joint prosthesis there was only 10-15
Service life, cannot meet long-time service require.Meanwhile infection is still one of catastrophic postoperative complications of orthopaedics implant.
The metallic foreign body to implant is the risk factor for causing such infection to occur, and a series of internal reactions caused include macrophage
The decrease of cell function, passivation of local immune system etc. are all that the proliferation of pathogen creates convenient condition.In addition, implantation
The albumen of object adsorption can also promote bacterial adhesion to cause infection to implant surface.Past people mostly concern to environment and
The removing of individual's pollution and the application of average of operation periods systemic antibiotics, and new method is the special mechanism for such infection morbidity
The risk of infection is reduced by implant surface modification.
The calcium phosphorous compounds such as hydroxyapatite and tricalcium phosphate can promote the combination of basis material and bone tissue, at
Ostosis, calcium phosphorous compound can gradually degrade, and then, calcium ion and phosphate anion are discharged into peripheral region, increase implantation
The deposition rate of object surface biological apatite, and lead to the knitting of bone regeneration around implant.
Metal material is considered to have biologically inert all the time, is modified although people have carried out various surfaces to its surface
Work come improve its activity, but the adherency of osteocyte growth it is still undesirable.And it is numerous research shows that magnesium have bioactivity,
Such as can induce cell differentiation, growth and blood vessel are grown into, after the implant devices implantation organism, osteocyte to magnesium by
Step is degraded and the space of reduction proliferation, differentiation, gradually forms new cancellous bone and cortex bone from inside to outside, and is had original strong
Degree and function, it is suitable for the nail bone plate etc. of fracture fixation, achievees the purpose that repair wound and Reconstruction of The Function.Meanwhile metal material
Magnesium (Mg) in material, because it has relatively negative corrosion potential, it is easy to chemical reaction occur with body fluid and degrade, by human body
It absorbs and is metabolized.Further, since the alkaline environment that magnesium is degraded and formed can achieve the purpose that inhibit implantation surrounding bacterial growth.
Invention content
The purpose of the present invention is to solve the synosteosis and infection problems of implantation material, and the present invention provides a kind of plants of bone
Enter with calcium phosphorous compound-magnesium composite coating and preparation method thereof, using bionical sedimentation and evaporation coating technique, titanium or titanium alloy,
Calcium phosphorous compound-magnesium composite coating is prepared on cobalt-base alloys, stainless steel, is asked with solving existing implantation material bone active and infection
Topic, this method gained Permanent implantation material is suitble to a variety of implant site mechanical property requirements, and has splendid biocompatibility, together
When have sterilizing function.
The present invention provides a kind of bone implantation calcium phosphorous compound-magnesium composite coatings, it is characterised in that：The calcium-phosphorus ratio
The thickness for closing object-magnesium composite coating is 6-220 μm.The range of coat thicknesses of wherein calcium phosphorous compound is：5-20μm；Magnesium coating
Thickness range is：1-200μm.
A kind of preparation method of bone implantation calcium phosphorous compound-magnesium composite coating, it is characterised in that：For calcium phosphorous compound
Coating is carrying out alkali Grape berry by NaOH first, and being then placed on matrix has the function of to accelerate calcium phosphorous compound deposition
Solution in bionical deposition, finally deposit calcium phosphorous compound at a certain temperature；For magnesium coating, pure magnesium is steamed using vapour deposition method
Hair, magnesium vapor can diffuse to the matrix position of calcium phosphorous compound, and deposited on its surface and obtain magnesium coating.
Matrix used is metalwork, is made of titanium or titanium alloy, cobalt-base alloys, stainless steel material.
Entity matrix used is medical material and device.
With the solution for accelerating calcium phosphorous compound to deposit function, 100-300mM/L containing NaCl, CaCl2 1-10mM/L,
NH4H2PO41-10mM/L and trishydroxymethylaminomethane (TRIS) 10-100mM/L, pure magnesium raw material are that Chun Du≤99.99% is pure
MAG block body.
The thickness of calcium phosphor coating is controlled by controlling sedimentation time, or by controlling pure magnesium evaporating temperature, depositing temperature, work
Make air pressure and sedimentation time to control the thickness of pure magnesium coating.
Bionical deposition method temperature is 50-90 DEG C；Pure magnesium evaporating temperature is 600-800 DEG C, depositing temperature 150-300
DEG C, deposition vacuum degree is 5-200Pa.
Specific preparation process is as follows：
(1), after using acetone, absolute ethyl alcohol and deionized water to be cleaned by ultrasonic successively matrix, it is put into a concentration of 1-5mol/L
NaOH solution in, 60-90 DEG C heat preservation 12-24h；
(2), 100-300mM/L containing NaCl, CaCl are prepared2 1-10mM/L,NH4H2PO41-10mM/L and trihydroxy methyl
Aminomethane (TRIS) 10-100mM/L's has the solution for accelerating calcium phosphorous compound deposition function；
(3) 0.5-1h is cleaned again with ultrasonic cleaning instrument after flushing three times the complete rear matrix of alkali heat with deionized water, finally will
Cleaned matrix is placed in the above-mentioned deposition solution at a temperature of 50-90 DEG C and deposits 6-12h；
(4), the pure MAG block of 1-50g is put into vaporization chamber target location, the matrix with calcium phosphor coating of drying is positioned over
Position from evaporation source 200-500mm, is evacuated to 10-3Pa hereinafter, cleaned minimum 3 times, to remove sky repeatedly with high-purity argon gas
Gas ensures oxygen-free environment；
(5), vaporization chamber is warming up to 600-800 DEG C of evaporating temperature, and MAG block evacuator body is that magnesium vapor spreads and is deposited on base
Body surface face, deposition cool to room temperature with the furnace after the completion.
Advantages of the present invention：
The present invention proposes a kind of bone implantation calcium phosphorous compound-magnesium composite coating, utilizes the bone-forming effect of calcium phosphorous compound
Alkaline environment after degrading with magnesium plays the role of local bactericidal, can promote osteocyte using the Biofunctional of magnesium ion
Growth.
Magnesium metal of the present invention has good bioactivity.Using the special self-bone grafting advantage of magnesium, bone tissue is gradually
The vacancy of magnesium after filling degradation, the degradation inducting osseous tissue and blood vessel of magnesium and calcium phosphorous compound are grown in matrix surface, to carry
The synosteosis ability of high matrix and tissue；The alkaline environment of magnesium coating degradation has bactericidal effect, makes the incidence of postoperative infection
It reduces, the success rate of operation is improved.
The method of prepares coating proposed by the present invention can coat certain thickness calcium phosphorus on a variety of orthopedic implanting material surfaces
Compound-magnesium composite coating is suitable for a variety of surfaces, and specially treated need not be carried out to material surface, applied widely.
Carrying out the processing of magnesium coating on different base surface makes implant surface have good bioactivity.Magnesium is in body fluid
Corrodible degradation.Calcium phosphorous compound can promote the combination of planting body and bone to varying degrees.Meanwhile magnesium belongs to normal in human body
Secondary element, content account for the 4th in all elements in vivo, play the role of to human metabolism very important.
Description of the drawings
Below in conjunction with the accompanying drawings and embodiment the present invention is described in further detail：
Fig. 1 is depositing device schematic diagram in embodiment 1.In figure, 1 settling chamber's furnace body；2 vaporization chamber furnace bodies；3, matrix；4, it steams
It rises；5, exhaust gas processing device；6, vacuum system；7, flow controller.
Fig. 2 a, b are surface and the section electron micrograph of embodiment 1 respectively.
Fig. 3 a, b are surface and the section electron micrograph of embodiment 2 respectively.
Fig. 4 a, b are respectively the front and back sample X-ray diffractogram of Examples 1 and 2 deposition.In figure, abscissa is 2 θ of the angle of diffraction
(degree), ordinate are intensity (A.U.).
Fig. 5 a, b, c are respectively material surface photomacrograph after embodiment 4 is impregnated 3,7,14 days with Hanks '.
Fig. 6 a, b, c are respectively that Titanium base and 5 staphylococcus aureus of embodiment co-culture the bacterium colony counting tablet photograph after 3h
Piece and example 6 are implanted into synosteosis situation of the new zealand white rabbit mandibular after 3 months.
Specific implementation mode
As shown in Figure 1, the depositing device used in the method for the present invention includes：Settling chamber's furnace body 1, vaporization chamber furnace body 2 etc., heavy
Matrix is placed in product room furnace body 1, evaporation source 4, one end of evaporation source 4 and the one of flow controller 7 are placed in vaporization chamber furnace body 2
End connection, the other end of flow controller 7 are separately connected H2With Ar supply lines, where the other end and matrix of evaporation source 4
Settling chamber communicates, and the settling chamber where matrix is communicated with exhaust gas processing device 5 and vacuum system 6 respectively.
It is evaporation source that the present invention, which uses physics vapour deposition system prepares coating, blocky pure magnesium, controls deposition position and steaming
Distance between origination location, equipment drawing are as shown in Figure 1.Matrix sample need to be washed through pickling, after alcohol washes, dry nitrogen air-blowing
It is dry, then it is placed in settling chamber's furnace body 1.
Embodiment 1
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 3mol/L and keeps the temperature for 24 hours for 80 DEG C；Then 100mM/L containing NaCl, CaCl are prepared2
3mM/L,NH4H2PO42mM/L's and trishydroxymethylaminomethane (TRIS) 50mM/L has the function of to accelerate calcium phosphorous compound deposition
Solution；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix is placed in the above-mentioned deposition solution at a temperature of 50 DEG C and deposits 12h.As shown in Fig. 2, the calcium phosphor coating prepared is in mainly tile
Shape simultaneously shows porous surface, and the thickness of coating is 20 μm or so.Its X-ray diffraction spectrum as shown in fig. 4 a, calcium phosphorous compound
Composition is mainly hydroxyapatite (HA) and tricalcium phosphate (OCP).
Embodiment 2
Matrix sample with calcium phosphor coating prepared by the example 1 of drying is placed in settling chamber's furnace body 1, pure MAG block is put into
The matrix with calcium phosphor coating of drying prepared is positioned over the position from evaporation source 300mm by vaporization chamber target location,
It is evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee oxygen-free environment repeatedly with high-purity argon gas.Pure magnesium evaporation
Temperature is 600 DEG C, working vacuum degree 5Pa, sets 150 DEG C, sedimentation time 0.5h of depositing temperature, and MAG block is evaporated to magnesium vapor diffusion
And it is deposited on matrix surface, room temperature is cooled to the furnace after the completion of reaction.As shown in Figure 3.Deposited metal magnesium coating by big
The pure magnesium composition of grain, it is 1 μm or so to have certain gap, magnesium coating layer thickness between particle and particle, the thickness of total composite coating
Degree is 21 μm or so.
Embodiment 3
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 1mol/L and keeps the temperature for 24 hours for 80 DEG C；Then 120mM/L containing NaCl, CaCl are prepared2
3mM/L,NH4H2PO44mM/L's and trishydroxymethylaminomethane (TRIS) 50mM/L has the function of to accelerate calcium phosphorous compound deposition
Solution；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix, which is placed in the above-mentioned deposition solution at a temperature of 50 DEG C, deposits 8h, and the calcium phosphor coating thickness of preparation is 10 μm or so.By pure magnesium
Block is put into vaporization chamber target location, and the matrix with calcium phosphor coating of drying prepared is positioned over from evaporation source 300mm
Position, be evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee oxygen-free environment repeatedly with high-purity argon gas.It is pure
Magnesium evaporating temperature is 750 DEG C, working vacuum degree 10Pa, sets 300 DEG C of depositing temperature, sedimentation time 0.5h, MAG block is evaporated to magnesium
Steam spreads and is deposited on matrix surface, and room temperature is cooled to the furnace after the completion of reaction.Magnesium coating layer thickness is 1 μm or so, total
The thickness of composite coating is 6 μm or so.
Embodiment 4
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 1mol/L and keeps the temperature for 24 hours for 80 DEG C；Then 120mM/L containing NaCl, CaCl are prepared2
3mM/L,NH4H2PO44mM/L's and trishydroxymethylaminomethane (TRIS) 50mM/L has the function of to accelerate calcium phosphorous compound deposition
Solution；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix, which is placed in the above-mentioned deposition solution at a temperature of 50 DEG C, deposits 8h, and the calcium phosphor coating thickness of preparation is 10 μm or so.By pure magnesium
Block is put into vaporization chamber target location, and the matrix with calcium phosphor coating of drying prepared is positioned over from evaporation source 300mm
Position, be evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee oxygen-free environment repeatedly with high-purity argon gas.It is pure
Magnesium evaporating temperature is 750 DEG C, working vacuum degree 10Pa, sets 300 DEG C of depositing temperature, sedimentation time 1.5h, MAG block is evaporated to magnesium
Steam spreads and is deposited on matrix surface, and room temperature is cooled to the furnace after the completion of reaction.As shown in Figure 3.Deposited metal magnesium coating
Be made of the pure magnesium of bulky grain, have certain gap between particle and particle, magnesium coating layer thickness is 60 μm or so, and total is compound
The thickness of coating is 70 μm or so.Its X diffraction spectra is as shown in Figure 4 b, it is seen that surface is mainly pure magnesium, and thickness is thicker, diffraction spectra
In only magnesium exist.It does not fall off from matrix in implantation process floating coat to confirm, has carried out immersion test, result is as schemed
Shown in 5, coating does not fall off from matrix still after impregnating 3 days, 7 days and 14 days respectively.In order to determine the anti-microbial property of coating, by band
Coating sample is according to " JIS Z 2801-2000《Antibacterial fabricated product-antibiotic property test method and antibacterial effect》、GB/T
2591-2003《Antibiotic plastic anti-microbial property experimental method and antibacterial effect》" etc. correlation standards carry out quantitative antibiotic property
It can detection.As a result it is 99% to obtain the sterilizing rate after sample acts on staphylococcus aureus, and design sketch is as shown in Figure 6 b.
Embodiment 5
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 1mol/L and keeps the temperature for 24 hours for 80 DEG C；Then 120mM/L containing NaCl, CaCl are prepared2
3mM/L,NH4H2PO44mM/L's and trishydroxymethylaminomethane (TRIS) 50mM/L has the function of to accelerate calcium phosphorous compound deposition
Solution；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix, which is placed in the above-mentioned deposition solution at a temperature of 50 DEG C, deposits 8h, and the calcium phosphor coating thickness of preparation is 10 μm or so.By pure magnesium
Block is put into vaporization chamber target location, and the matrix with calcium phosphor coating of drying prepared is positioned over from evaporation source 300mm
Position, be evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee oxygen-free environment repeatedly with high-purity argon gas；It is pure
Magnesium evaporating temperature is 650 DEG C, working vacuum degree 20Pa, sets 200 DEG C, sedimentation time 1h of depositing temperature, and MAG block evacuator body is magnesium
Steam spreads and is deposited on matrix outermost, cools to room temperature with the furnace after the completion of reaction, the thickness of deposited metal magnesium coating is
50 μm or so, the thickness of total composite coating is 60 μm or so.In order to verify the biocompatibility of coating and promote bone growth spy
Property, the bar samples with composite coating are implanted into the mandibular of new zealand white rabbit, the combination interface of implant and bone after 3 months
As fig. 6 c.As seen from the figure, all degradation is complete substantially for magnesium coating and calcium phosphorous compound coating.
Embodiment 6
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 3mol/L and keeps the temperature for 24 hours for 80 DEG C；Then 130mM/L containing NaCl, CaCl are prepared2
3mM/L,NH4H2PO43mM/L's and trishydroxymethylaminomethane (TRIS) 40mM/L has the function of to accelerate calcium phosphorous compound deposition
Solution；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix, which is placed in the above-mentioned deposition solution at a temperature of 50 DEG C, deposits 6h, and the calcium phosphor coating thickness of preparation is 5 μm or so.By pure MAG block
It is put into vaporization chamber target location, the matrix with calcium phosphor coating of drying prepared is positioned over from evaporation source 300mm's
Position is evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee oxygen-free environment repeatedly with high-purity argon gas；Pure magnesium
Evaporating temperature is 750 DEG C, working vacuum degree 110Pa, sets 200 DEG C, sedimentation time 1.5h of depositing temperature, and MAG block is evaporated to magnesium steaming
Gas spreads and is deposited on matrix surface, cools to room temperature after the completion of reaction with the furnace, the thickness of deposited metal magnesium coating is 100 μm
Left and right.The thickness of obtained total calcium phosphorous compound-magnesium composite coating is 105 μm.
Embodiment 7
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 3mol/L and keeps the temperature for 24 hours for 70 DEG C；Then 150mM/L containing NaCl, CaCl are prepared2
4mM/L,NH4H2PO42mM/L's and trishydroxymethylaminomethane (TRIS) 50mM/L has the function of to accelerate calcium phosphorous compound deposition
Solution；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix, which is placed in the above-mentioned deposition solution at a temperature of 60 DEG C, deposits 12h, and the calcium phosphor coating thickness of preparation is 20 μm or so.By pure magnesium
Block is put into vaporization chamber target location, and the matrix with calcium phosphor coating of drying prepared is positioned over from evaporation source 300mm
Position, be evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee oxygen-free environment repeatedly with high-purity argon gas；It is pure
Magnesium evaporating temperature is 800 DEG C, working vacuum degree 200Pa, sets 250 DEG C, sedimentation time 2h of depositing temperature, and MAG block evacuator body is magnesium
Steam spreads and is deposited on matrix surface, cools to room temperature after the completion of reaction with the furnace, the thickness of deposited metal magnesium coating is 150
μm or so.Total coating layer thickness is 170 μm.
Embodiment 8
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 3mol/L and keeps the temperature for 24 hours for 80 DEG C；Then 120mM/L containing NaCl, CaCl are prepared2
2.5mM/L,NH4H2PO4Having for 3mM/L and trishydroxymethylaminomethane (TRIS) 40mM/L accelerates calcium phosphorous compound to deposit work(
The solution of energy；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix be placed in the above-mentioned deposition solution at a temperature of 50 DEG C and deposit 10h, the calcium phosphor coating thickness of preparation is 15 μm or so.It will be pure
MAG block is put into vaporization chamber target location, and the matrix with calcium phosphor coating of drying prepared is positioned over from evaporation source
The position of 300mm, is evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee anaerobic ring repeatedly with high-purity argon gas
Border；Pure magnesium evaporating temperature is 800 DEG C, working vacuum degree 200Pa, sets 300 DEG C, sedimentation time 2h of depositing temperature, and MAG block body steams
Hair is that magnesium vapor spreads and be deposited on matrix surface, and room temperature, the thickness of deposited metal magnesium coating are cooled to the furnace after the completion of reaction
Degree is 200 μm or so.Total composite coating thickness is 215 μm or so.
Embodiment 9
Sheet pure titanium (Ti) sample is polishing to 2000# with sand paper, uses acetone, absolute ethyl alcohol and deionized water ultrasound successively
After cleaning, it is put into the NaOH solution of a concentration of 3mol/L and keeps the temperature for 24 hours for 70 DEG C；Then 200mM/L containing NaCl, CaCl are prepared2
4mM/L,NH4H2PO4Having for 2mM/L and trishydroxymethylaminomethane (TRIS) 100mM/L accelerates calcium phosphorous compound to deposit work(
The solution of energy；1h is cleaned again with ultrasonic cleaning instrument after the complete rear matrix of alkali heat is flushed three times with deionized water, it finally will be cleaned
Matrix be placed in the above-mentioned deposition solution at a temperature of 60 DEG C and deposit 12h, the calcium phosphor coating thickness of preparation is 20 μm or so.It will be pure
MAG block is put into vaporization chamber target location, and the matrix with calcium phosphor coating of drying prepared is positioned over from evaporation source
The position of 300mm, is evacuated to 10-4Pa hereinafter, cleaned minimum 3 times, to remove air, guarantee anaerobic ring repeatedly with high-purity argon gas
Border；Pure magnesium evaporating temperature is 800 DEG C, working vacuum degree 150Pa, sets 200 DEG C, sedimentation time 2.5h of depositing temperature, MAG block body
It is evaporated to magnesium vapor and spreads and be deposited on matrix outermost, room temperature, deposited metal magnesium coating are cooled to the furnace after the completion of reaction
Thickness be 200 μm or so.Total coating layer thickness is 220 μm.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of bone implantation calcium phosphorous compound-magnesium composite coating, it is characterised in that：The compound painting of calcium phosphorous compound-magnesium
The thickness of layer is 6-220 μm.
2. the preparation method of bone implantation calcium phosphorous compound-magnesium composite coating described in a kind of claim 1, it is characterised in that：It is right
In calcium phosphorous compound coating, alkali Grape berry is being carried out by NaOH first, then matrix is being placed on acceleration calcium-phosphorus ratio
Bionical deposition in the solution of object deposition function is closed, finally deposits calcium phosphorous compound at a certain temperature；For magnesium coating, using steaming
Plating method evaporates pure magnesium, and magnesium vapor can diffuse to the matrix position of calcium phosphorous compound, and deposit and obtain on its surface
Obtain magnesium coating.
3. according to the preparation method of calcium phosphorous compound-magnesium composite coating of bone implantation described in claim 2, it is characterised in that：Institute
It is metalwork with matrix, is made of titanium or titanium alloy, cobalt-base alloys, stainless steel material.
4. according to the preparation method of calcium phosphorous compound-magnesium composite coating of bone implantation described in claim 3, it is characterised in that：Institute
It is medical material and device with entity matrix.
5. according to the preparation method of calcium phosphorous compound-magnesium composite coating of bone implantation described in claim 2, it is characterised in that：Tool
There are the solution for accelerating calcium phosphorous compound deposition function, 100-300mM/L containing NaCl, CaCl2 1-10mM/L,NH4H2PO4 1-
10mM/L and trishydroxymethylaminomethane (TRIS) 10-100mM/L, pure magnesium raw material are the pure MAG block body of Chun Du≤99.99%.
6. according to the preparation method of calcium phosphorous compound-magnesium composite coating of bone implantation described in claim 2, it is characterised in that：It is logical
The thickness of control sedimentation time control calcium phosphor coating is crossed, or by controlling pure magnesium evaporating temperature, depositing temperature, operating air pressure and sinking
The product time controls the thickness of pure magnesium coating.
7. according to the preparation method of calcium phosphorous compound-magnesium composite coating of bone implantation described in claim 2, it is characterised in that：It is imitative
Raw deposition method temperature is 50-90 DEG C；Pure magnesium evaporating temperature is 600-800 DEG C, and depositing temperature is 150-300 DEG C, and deposition is true
Reciprocal of duty cycle is 5-200Pa.
8. according to the preparation method of calcium phosphorous compound-magnesium composite coating of bone implantation described in claim 2, which is characterized in that tool
Preparation step is as follows：
(1), after using acetone, absolute ethyl alcohol and deionized water to be cleaned by ultrasonic successively matrix, it is put into a concentration of 1-5mol/L's
In NaOH solution, 60-90 DEG C of heat preservation 12-24h；
(2), 100-300mM/L containing NaCl, CaCl are prepared2 1-10mM/L,NH4H2PO41-10mM/L and trihydroxy methyl amino first
Alkane (TRIS) 10-100mM/L's has the solution for accelerating calcium phosphorous compound deposition function；
(3) 0.5-1h is cleaned again with ultrasonic cleaning instrument after flushing three times the complete rear matrix of alkali heat with deionized water, it finally will cleaning
Good matrix, which is placed in the above-mentioned deposition solution at a temperature of 50-90 DEG C, deposits 6-12h；
(4), the pure MAG block of 1-50g is put into vaporization chamber target location, the matrix with calcium phosphor coating of drying is positioned over from steaming
It rises the position of 200-500mm, is evacuated to 10-3Pa hereinafter, cleaned minimum 3 times repeatedly with high-purity argon gas, to remove air, is protected
Demonstrate,prove oxygen-free environment；
(5), vaporization chamber is warming up to 600-800 DEG C of evaporating temperature, and MAG block evacuator body is that magnesium vapor spreads and is deposited on matrix table
Face, deposition cool to room temperature with the furnace after the completion.
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| CN109457207A (en) * | 2018-11-22 | 2019-03-12 | 九江学院 | A kind of preparation method of hydroxylapatite-magnesium composite coating |
| CN109911873A (en) * | 2019-03-18 | 2019-06-21 | 浙江大学 | A kind of method of titanium implant surface assemble nanometer grade hydroxyapatite |
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