CN106620852A - Method for preparing dicalicium phosphate anhydrous (DCPA) bioceramic coating on surface of pure titanium - Google Patents
Method for preparing dicalicium phosphate anhydrous (DCPA) bioceramic coating on surface of pure titanium Download PDFInfo
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The invention discloses a method for preparing a dicalicium phosphate anhydrous (DCPA) bioceramic coating on the surface of pure titanium. The method comprises the following steps: preparing an aqueous solution of the DCPA, wherein the concentration of the aqueous solution is 0.05 to 0.25g/ml; carrying out hydrophilic pretreatment on a pure titanium substrate; heating the substrate under the condition of 50 to 100DEG C, and enabling the surface of the substrate to be dry; repeatedly and uniformly spraying the aqueous solution of the DCPA on the surface of the substrate. According to the method disclosed by the invention, liquid drops are refined by using a dissolution-separation principle and adopting a spraying method, and CaHPO4.2H2O is dehydrated at lower temperature to form the DCPA; the method is simple in preparation process, mild in reaction conditions and not high in safety requirement; meanwhile, according to a bioactive DCPA coating prepared on the surface of a metal matrix by adopting the method disclosed by the invention, the proportions of Ca/P elements are not changed; the coating is pure in phase, uniform and compact, and can completely cover a matrix; interaction between an implant and tissue cells can be adjusted, osteoblastic differentiation of stem cells is promoted, and the combinability of the implant and bone is improved.
Description
Technical field
The present invention relates to a kind of method that pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, belongs to Srgery grafting
Thing technical field.
Background technology
Pure titanium is the major metal material for manufacturing load bone implant, is that it is long-term, stable with combining closely for host bone
Play the premise of repair.But medical pure titanium is bio-inert material, after the product implantation human body directly manufactured by it easily
The problems such as appearance loosening, abrasion, fibr tissue intervention and infection, and bioactivity coatings are undoubtedly metal in guarantee human body environment
The approach the most feasible of the long-acting operation of implant.Hydroxyapatite (HAP) coating can become mesh due to good osteoconductive
The widest coating of metal implant surface applications in prebone, but HAP does not possess osteoinductive.As patient uses up to implant
The serious hope of early load and quick healing is more and more stronger, and preparing for the new bio coating with osteoinductive is urgently to be resolved hurrily.With
The higher HAP of chemical stability is compared, calcium monohydrogen phosphate (CaHPO4, DCPA) solubility it is higher, degradation rate is moderate, Neng Gou
Ca is formed at implant-bone interface2+、PO4 3-Supersaturation region, induces stem cell Osteoblast Differentiation (Habibovic P., et
al.Osteoconduction and osteoinduction of low-temperature3D printed bioceramic
implants.Biomaterials,2008,29:944-953.).As can be seen here, DCPA coatings hold promise as biology of new generation
Active coating is applied to metal intra-osseous implant surface.
The report for preparing DCPA bioactivity coatings on medical metal surface at present is still few, and the method found has following
It is several.Sensing heating is carried out to Titanium base in containing calcium, the solution of phosphonium ion and prepares DCPA coatings, electric current is 25A, due to base
Body surface face water acutely gasifies, and DCPA coatings prepared by this method are grown in the way of platelet cluster, fail that titanium-based is completely covered
Body (Kuroda K., et al.Preparation of calcium phosphate coatings on titanium
using the thermal substrate method and their in vitro evaluation.Materials
Transactions,2002,43:3015-3019).Prepared first on metallic matrix by chemical deposition, electrochemical deposition method
Dicalcium phosphate dihydrate (CaHPO4·2H2O), then again through heat treatment prepare DCPA coatings, in the method element ratio control compared with
Difficulty, is mingled with calcium pyrophosphate and weakens its biocompatibility (Li K., et al.Microstructure, in vitro in final product
corrosion and cytotoxicity of Ca-P coatings on ZK60magnesium alloy prepared
by simple chemical conversion and heat treatment.Journal of Biomaterials
Applications,2013,28:375-84).Further, it is also possible to prepare DCPA coatings, this method by sol-gel process
Operation difficulty is larger, take it is more, and be easily mingled with DCPA coatings the impurity such as calcium carbonate (Eshtiagh-Hosseini H.,
et al.Preparation of anhydrous dicalcium phosphate,DCPA,through sol–gel
process,identification and phase transformation evaluation.Journal of Non-
crystalline Solids,2008,354:3854-3857).In sum, the DCPA coating production masters being currently known
Suffer from the drawback that：(1) equipment is complicated, and security performance has high demands；(2) high current or high temperature are needed (more than 100 DEG C).Operation；
(3) the DCPA coatings prepared by can not be completely covered matrix or there is impurities phase；(4) working environment is poor, and efficiency is low, energy consumption
Greatly.
The content of the invention
Goal of the invention：It is an object of the invention to provide one kind can prepare osteoinductive DCPA on medical pure Titanium base surface applying
The method of layer, to shortening implant and host bone healing cycle, improves implant synosteosis.
Technical scheme：Preparation method of the present invention, comprises the steps of：(1) the DCPA aqueous solution is prepared, concentration is
0.05-0.25g/ml；(2) pure Titanium base hydrophiling pretreatment；(3) heating pure Titanium base under the conditions of 50-100 DEG C makes its table
Face is dried；(4) by the DCPA aqueous solution repeatedly even application in pure Titanium base surface.
Wherein, the entitled calcium phosphate dibasic anhydrous of DCPA Chinese.
Preferably, in step (1), the concentration for preparing the DCPA aqueous solution is 0.1-0.2g/ml, to ensure effect prepared by coating
Rate and quality of forming film；Deionized water and effumability acid are added DCPA aqueous solution process is prepared：On the one hand, DCPA is in deionization
Solubility in water is very low, and acid adding can reduce pH, increases DCPA meltages；On the other hand, in the drying that subsequently may be carried out
During, this kind of acid can be easy to vapor away, and noresidue does not affect coating purity；Meanwhile, these effumability acid are concentration
The hydrochloric acid of 0.05-0.25mol/L, can realize above-mentioned purpose；Further, need to add 0.08mol/ per 0.1g/ml DCPA
The HCl of L, as often as possible dissolves DCPA, and maximum plays the effect of HCl；Additionally, DCPA is to analyze more than pure.
Pure Titanium base in step (2) is the pure titanium of implanted medical device, i.e. CP- titaniums, need to meet ISO5032 and
ASTMF67 is required.The hydrophiling pretreatment carried out to pure Titanium base is extremely important, after can causing solution spraying to sample
It is even to be covered in its surface, can guarantee that spraying uniformity, coatings growth uniformity；If not carrying out hydrophilicity-imparting treatment, solution may
Aggregation becomes one by one or several big drops, postpones drying time, and causes coating from homoepitaxial.The present invention can
Realize that hydrophiling is located in advance by the irradiation of acid etching, sandblasting-acid etching, alkali heat-treatment, corona treatment, hydro-thermal process or ultraviolet
Reason.Before this step, sand papering and ultrasonic wave cleaning generally can be carried out to matrix sample, scavenging period can be controlled
10min or so, the medium of cleaning is generally followed successively by absolute ethyl alcohol or acetone, pure water, and is dried, to remove bruting process in adhere to
In the greasy dirt on surface.
In step (3), pure Titanium base is easily operated under the conditions of 50-100 DEG C, if being less than 50 DEG C, can not filled because of dehydration
It is mitogenetic into DCPD constituent phases, and more than 120 DEG C after DCPA can decompose；Preferable temperature is 70-80 DEG C, moderate drying speed, it is ensured that
Coating efficiency.In addition, the heater for being used can be the one kind in constant temperature electric heating case, electric calorifier, electric stage.
In step (4), spraying means be it is crucial, needs accomplish spraying it is uniform, it is a small amount of repeatedly, every time spraying should keep away from
It is consistent from, angle, intensity, it is to avoid matrix surface forms obvious drop aggregation, or there is the area not covered by solution in matrix surface
Domain.Spray should be to carry out under normal temperature, it is also possible to carries out under conditions of step (3).Spraying number of times is have to the quality of coating
Affected, when COPA concentration be 0.1-0.2g/ml when, spray for 40-60 effect it is preferable.Meanwhile, every time to pure Titanium base
Its dry tack free is confirmed before spraying.It is furthermore preferred that after last time is sprayed, then the pure Titanium base is dried into more than 30 minutes
Take out, preserve after cooling.Additionally, spraying, such as manual sealing spraying, electric atomizing or motor-driven spray can be realized using sprayer unit
Mist device etc..
Beneficial effect：Compared with prior art, remarkable advantage of the invention is：Using the principle of crystallization of the dissolution and precipitation, using spray
Mist method refines drop, makes CaHPO4·2H2O is dehydrated to form DCPA at relatively low temperature, and preparation process is simple, reacts bar
Part is gentle, is not related to high current or high-temperature operation, and security requirement is not high, and operability is greatly improved, and working environment is good
It is good, it is adapted to laboratory or medicine equipment cleaning shop uses；Meanwhile, the life prepared in metal base surface using the inventive method
Thing activity DCPA coatings, do not change Ca/P element ratios, and coating substance is mutually single, even compact, matrix can be completely covered and can adjust
Reciprocation between implant and histocyte, promotes stem cell Osteoblast Differentiation, improves implant synosteosis.
Description of the drawings
Fig. 1 is surface microscopic topographic after the pure Titanium base acid corroding pretreatment of the embodiment of the present invention 1；
Fig. 2 is the microscopic appearance that the embodiment of the present invention 1 is obtained coating；
Fig. 3 is the XRD analysis result of the matrix of the embodiment of the present invention 1 and prepared coating；
Fig. 4 is the microscopic appearance that the embodiment of the present invention 2 is obtained coating；
Fig. 5 is the XRD analysis result of the matrix of the embodiment of the present invention 2 and prepared coating；
Fig. 6 is the microscopic appearance that the embodiment of the present invention 3 is obtained coating；
Fig. 7 is the XRD analysis result of the matrix of the embodiment of the present invention 3 and prepared coating.
Specific embodiment
Technical scheme is described further below in conjunction with the accompanying drawings.
Embodiment 1
5g is weighed with electronic balance and analyze pure DCPA powder, in being transferred to glass beaker, add 96mL deionized waters, addition
4moL concentration is the watery hydrochloric acid HCl of 0.04mol/L, is stirred with glass bar, treats CaHPO4After being completely dissolved, solution is transferred to
In PET tying spray bottles.The pure titanium that sand papering and ultrasonic wave were cleaned is placed in 70 DEG C of hydrochloric acid-sulfuric acid mixed solution and is located
Reason 30 minutes, uses afterwards a large amount of deionized water rinsings, acquisition to possess the acid etching surface of Superhydrophilic.Pure Titanium base is put into constant temperature
In resistance box, temperature setting is 50 DEG C, after being incubated 5 minutes, confirms that matrix surface is completely dried.Press atomizing pump so that DCPA
Solution is uniformly sprayed on Titanium base, and because matrix is Superhydrophilic, DCPA solution can uniformly be sprawled on its surface.For the first time
After spraying, about 30 seconds are incubated, matrix surface carries out again second spraying after being completely dried, such spraying-drying-spraying, repeatedly
120 times.After last time is sprayed, insulation takes out sample after 30 minutes, cools down, and preserves.
Table is carried out to the matrix surface of the above-mentioned process of Jing with SEM (SEM) and X-ray diffractometer (XRD)
Levy, as a result as shown in Figure 1, Figure 2, Figure 3 shows.XRD results show, Jing after above-mentioned process, in addition to the diffraction maximum of pure Titanium base, occur
New diffraction maximum, and their corresponding exactly DCPA, do not find in addition other peaks, it is seen that matrix surface does not have in addition to DCPA
There is other impurities phase.SEM observation indicate that, although the DCPA prepared with this method can be completely covered Titanium base, particle
Tiny, the coarse profile of matrix surface is still visible.
Embodiment 2
Step is basically identical with embodiment 1, and difference is that this spray solution proportioning is：25g analyzes pure DCPA,
80ml deionized waters, 20mL concentration is the watery hydrochloric acid HCl of 0.20mol/L.It is 30 times that spraying is dried number of times, 60 DEG C of baking temperature.
SEM (Fig. 4), XRD (Fig. 5) analysis result show that the DCPA coating uniforms prepared with this method are complete, and titanium-based can be completely covered
Body.
Embodiment 3
Step is basically identical with embodiment 1, and difference is that this spray solution proportioning is：10g analyzes pure DCPA,
92ml deionized waters, 8mL concentration is the watery hydrochloric acid HCl of 0.08mol/L.It is 60 times that spraying is dried number of times, 70 DEG C of baking temperature.
SEM (Fig. 6), XRD (Fig. 7) analysis result show that the DCPA coating uniforms prepared with this method are complete, fine and close, can be completely covered
Titanium base.
Reference examples 1
Step is basically identical with embodiment 3, and difference is that this spray solution proportioning is：(1) 2g analyzes pure DCPA,
100ml deionized waters, without acid, now DCPA has reached maxima solubility wherein in deionized water.SEM is observed not
Can find that titanium specimen surface has obvious deposit.
Reference examples 2
Step is basically identical with embodiment 3, and difference is that this spray solution proportioning is：30g analyzes pure DCPA,
76ml deionized waters, 24mL concentration is the watery hydrochloric acid HCl of 0.24mol/L.SEM observations find the deposit of specimen surface to disperse
Wad shape is present, and fails to form uniform coating.
Reference examples 3
Step is basically identical with embodiment 3, and it is 40 DEG C that difference is baking temperature.SEM observations find specimen surface
Deposit present flaky crystal shape, XRD analysis are DCPD, fail with matrix formed combine closely.
Reference examples 4
Step is basically identical with embodiment 3, and it is 200 DEG C that difference is baking temperature.SEM observations find specimen surface
Deposit be scattered rhombus bulk crystals, XRD analysis are calcium pyrophosphate.
Reference examples 5
Step is basically identical with embodiment 3, and it is 80 DEG C that difference is baking temperature.SEM is it has been observed that DCPA coatings
Completely, Titanium base can be completely covered, particle size uniformity, arrangement are fine and close.
Reference examples 6
Step is basically identical with embodiment 3, and it is 75 DEG C that difference is baking temperature.SEM is it has been observed that DCPA coatings
Completely, Titanium base can be completely covered, particle size uniformity, arrangement are fine and close.
Reference examples 7
Step is basically identical with embodiment 3, and it is 100 DEG C that difference is baking temperature.SEM it has been observed that
DCPA coatings can be completely covered surface, but granular size is uneven, arrange more loose.
Reference examples 8
Step is basically identical with embodiment 3, and it is 150 DEG C that difference is baking temperature.SEM is it has been observed that circular
Grain is mixed with arrangement with square water chestnut shape crystal grain, that is, define calcium pyrophosphate, and coating fails that matrix is completely covered.
Reference examples 9
Step is basically identical with embodiment 3, and it is 20 times that difference is spraying number of times.SEM observes visible specimen surface
A large amount of graininess deposits, size is uneven, and fails that sample is completely covered.
Reference examples 10
Step is basically identical with embodiment 3, and it is 80 times that difference is spraying number of times.SEM observes visible specimen surface
There are a large amount of graininess deposits, sample can be completely covered, but surface particles are presented lint shape, and coating is more open.
Reference examples 11
Step is basically identical with embodiment 3, and it is that not hydrophilic treated sand paper is beaten that difference is used matrix
Mill sample.SEM observes visible specimen surface a large amount of particles, but its size and be distributed it is very uneven, segregation in the edge of sample,
Fail to form uniform coating.
Now the process and result of above-described embodiment and reference examples are aggregated into table 1：
The embodiment of table 1 and reference examples collect
From above-described embodiment, solution concentration affects film forming efficiency and quality.Without during acid, DCPA dissolvings are spent
It is low, even if through repeatedly spraying, still can not be in specimen surface into coating；With the raising of DCPA concentration, coating granule is gradually
Increase, 0.1g/ml (or 100g/L) left and right more uniform and delicate effect is best.When spraying number of times is less, particle size is uneven
And can not form complete coating, and spray number of times it is more when, particle surface is presented lint shape, and coating is loose.Baking temperature affects
Coating final thing phase composition, low temperature does not easily thoroughly form DCPD because of dehydration, and high temperature is easily caused and is decomposed to form calcium pyrophosphate.Separately
Outward, it is also to ensure DCPA uniformly into the important prerequisite of coating that surface hydrophilic is processed.
Claims (10)
1. a kind of method that pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that comprise the steps of：
(1) the DCPA aqueous solution is prepared, concentration is 0.05-0.25g/ml；
(2) pure Titanium base hydrophiling pretreatment；
(3) heating pretreated pure Titanium base under the conditions of 50-100 DEG C makes its dry tack free；
(4) by the DCPA aqueous solution repeatedly even application in pure Titanium base surface.
2. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
In step (1), the concentration for preparing the DCPA aqueous solution is 0.1-0.2g/ml.
3. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
In step (4), the spraying is carried out at normal temperatures.
4. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
In step (3), the pure Titanium base is heated under the conditions of 70-80 DEG C.
5. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
In step (1), the DCPA aqueous solution is prepared using deionized water and effumability acid.
6. the method that according to claim 5 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
The effumability acid is the hydrochloric acid of concentration 0.05-0.25mol/L.
7. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
In step (1), the DCPA is the pure CaHPO above of analysis4Or CaHPO4·2H2O。
8. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
In step (2), the hydrophiling pretreatment that the pure Titanium base is carried out includes acid etching, sandblasting-acid etching, alkali heat-treatment, plasma
Process, hydro-thermal process or ultraviolet are irradiated.
9. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, it is characterised in that：
In step (4), every time to confirming its dry tack free before the spraying of pure Titanium base.
10. the method that according to claim 1 pure titanium surface prepares calcium phosphate dibasic anhydrous bio-ceramic coating, its feature exists
In：In step (4), after last time is sprayed, the pure Titanium base is dried, then takes out and preserved after cooling.
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| CN108531893A (en) * | 2018-04-04 | 2018-09-14 | 天津大学 | A kind of microwave preparation of Mg alloy surface nano whiskers calcium monohydrogen phosphate coating |
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