CN102851664B - Method for preparing hydroxy apatite biological ceramic coating containing fluorine - Google Patents
Method for preparing hydroxy apatite biological ceramic coating containing fluorine Download PDFInfo
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Abstract
The invention discloses a method for preparing a hydroxy apatite biological ceramic coating containing fluorine. The method comprises the steps of evenly mixing 2.3% of calcium fluoride powder by weight and 97.7% of hydroxyapatite powder by weight, utilizing polyving akohol solution with concentration of 2% to serve as binder to allocate the mixed powder, presetting the allocated mixed powder on a titanium alloy base plate, and utilizing a carbon dioxide laser to perform broadband laser cladding on the titanium alloy base plate to generate the hydroxy apatite biological ceramic coating containing the fluorine, wherein the cladding process adopts two process parameters as follows: the laser output power P of the carbon dioxide laser ranges from 0.5kW to 1kW, the scanning speed V ranges from 150nm/min to 250nm/min, the rectangular spot dimension D is 15mm*2mm, and argon shield is adopted. By means of the method, good biological activity of the ceramic coating and high strength and good toughness of metal are combined together, and the hydroxy apatite coating containing the fluorine can protect the titanium alloy base plate from being corroded by the human physiological environment. Besides, the coating and the metal of the base plate are combined through the laser cladding preparation technique, so that the hydroxy apatite biological ceramic coating containing the fluorine meets mechanical performance requirements of implant materials.
Description
Technical field
The invention belongs to bio-ceramic coating Material Field, more specifically, relate to a kind of method of preparing Hydroxy-Fluor-Apatite Bioceramics coating.
Background technology
Synthetic biomaterial is of a great variety, and titanium and alloy thereof and hydroxyapatite are all widely used in the research and development of biomedical material as the best metallic substance of biological activity and stupalith respectively.The former is because the corrosion under human body environment produces the atoms metal of toxic side effect, and the latter has limited their application because fragility is large, intensity is low.Hydroxyapatite coating layer has higher solubleness, this can reduce its stability and the long-term performance of implanting, fluoridated hydroxyapatite more approaches the composition of natural bone owing to utilizing F-to replace OH-, can effectively improve the biological activity of hydroxyapatite and there is lower solubleness, having become the main biological activity bone substitution material of Clinical Selection.
Laser melting coating biological ceramics technology refers under the micro-molten condition of base material, adopts high energy laser beam by the biological ceramic powder fusing that is preset in metallic substrate surface or synchronously sends into, and obtains Bioceramic Composite.Comparing with traditional spraying coating process, is metallurgical binding between the cladding layer of laser melting coating and base material, and bonding strength is higher, and laser cladding process can accurately control, and easily realizes automatization.
Patent CN 1778989A discloses a kind of synthetic method of preparing Bioceramic Composite of Laser Cladding in-situ, utilize high energy laser beam to carry out laser melting and coating process processing to calcium salt composite powder and metal substrate, make calcium salt composite powder reaction in－situ generate hydroxyapatite P and β-Ca
2p
2o
7composite boilogical ceramic coating for main component.
Patent CN 1087807A discloses a kind of manufacture method of high-purity fluorine apatite biological painting, and high-purity fluorine apatite powder is added to appropriate forming machine, through mold pressing, isostatic cool pressing, after sintering, can make high-purity fluorine Apatite Ceramic.The high-purity fluorine apatite powder that adopts sol-gel technique to make, high-temperature stability is good, is adapted to pass through high temperature sintering and prepares active biological ceramic.
At present, adopt laser melting and coating technique to prepare the biological coating of multiple hydroxyl phosphatic rock, and the preparation of fluoridated hydroxyapatite coating still be take sol-gel method and plasma spraying method as main, coating and substrate bonding strength are lower, even occur peeling off, falling the situations such as piece.
Summary of the invention
Defect for prior art, the object of the present invention is to provide a kind of method of preparing Hydroxy-Fluor-Apatite Bioceramics coating, be intended to solve in prior art hydroxyapatite permanent stability poor, rate of decomposition is fast, and sol-gel method, the problem such as anchoring strength of coating prepared by the methods such as plasma spraying method is low, adopt laser cladding method on titanium alloy substrate, to prepare containing Hydroxy-Fluor-Apatite Bioceramics coating, on the one hand by the good biological activity of ceramic coating and the high strength of metal, good toughness combination together, and make fluoridated hydroxyapatite coating have the effect that protection titanium alloy substrate is avoided Human Physiology environmental corrosion concurrently, utilize on the other hand laser melting coating technology of preparing to make coating and substrate produce good metallurgical binding, meet the mechanical property requirements of embedded material.
For achieving the above object, the invention provides a kind of method of preparing Hydroxy-Fluor-Apatite Bioceramics coating, comprise the following steps:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix;
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate;
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate; to generate Hydroxy-Fluor-Apatite Bioceramics coating; the processing parameter that cladding process adopts is: carbon dioxide laser laser output power P=0.5-1kW; scan velocity V=150-250mm/min; rectangular light spot dimension D=15mm * 2mm, and adopt argon shield.
In step (1), be to adopt ball mill that mixed powder is carried out ball milling refinement and evenly mixed.
In step (3), be to utilize manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
The present invention also provides a kind of method of preparing Hydroxy-Fluor-Apatite Bioceramics coating, comprises the following steps:
The Calcium Fluoride (Fluorspan) powder that (1 ') is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix;
(2 ') utilizes concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3 ') is preset at deployed mixed powder on titanium alloy substrate;
(4 ') adopts optical fiber laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating, the processing parameter that cladding process adopts is: optical fiber laser laser power 0.8-1kw, sweep velocity 720mm/min, tabula rasa size
and adopt argon shield.
In step (1 '), be to adopt ball mill that mixed powder is carried out ball milling refinement and evenly mixed.
In step (3 '), be to utilize manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
The above technical scheme of conceiving by the present invention, compared with prior art, there is following beneficial effect: it is raw material that CaF2 and hydroxyapatite powder are take in the present invention, utilize laser melting and coating technique to obtain the Hydroxy-Fluor-Apatite Bioceramics coating of expected structure and performance, coating and substrate bonding strength are high, for chemical metallurgy combination, not only reduced the cost of manufacture of coating but also improved the bonding strength between coating and substrate.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The method that an embodiment of the present invention is prepared Hydroxy-Fluor-Apatite Bioceramics coating comprises the following steps:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, be to adopt ball mill that mixed powder is carried out ball milling refinement and evenly mixed;
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate; Particularly, be to utilize manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm;
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate; to generate Hydroxy-Fluor-Apatite Bioceramics coating; the processing parameter that cladding process adopts is: carbon dioxide laser laser output power P=0.5-1kW; scan velocity V=150-250mm/min; rectangular light spot dimension D=15mm * 2mm, and adopt argon shield.
The method that the another kind of embodiment of the present invention prepares Hydroxy-Fluor-Apatite Bioceramics coating comprises the following steps:
The Calcium Fluoride (Fluorspan) powder that (1 ') is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, be to adopt ball mill that mixed powder is carried out ball milling refinement and evenly mixed;
(2 ') utilizes concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3 ') is preset at deployed mixed powder on titanium alloy substrate; Particularly, be to utilize manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm;
(4 ') adopts optical fiber laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating, the processing parameter that cladding process adopts is: optical fiber laser laser power 0.8-1kw, sweep velocity 720mm/min, tabula rasa size
and adopt argon shield.
Example 1:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=0.5kW, and scan velocity V=200mm/min, spot size D=15mm * 2mm, and adopt argon shield.Now, because laser power is lower, the laser energy absorbing in sample unit surface is lower, causes the fusing of coating and substrate surface insufficient, is not enough to form molten bath at titanium alloy surface, does not form bio-ceramic coating.
Example 2:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=0.7kW, and scan velocity V=200mm/min, spot size D=15mm * 2mm, and adopt argon shield.Now, substrate surface forms continuous coated, and coating is that chemical metallurgy is combined with substrate, and the microhardness maximum of ceramic layer is 1202HV
0.2, illustrate and under these processing condition, utilize laser melting and coating technique to obtain to be combined with substrate good ceramic coating.The thing of Hydroxy-Fluor-Apatite Bioceramics coating is mutually mainly by Al
3v, TiO
2, CaF
2, Ca
3(PO
4)
2xH
2o and Ca
5(PO
4)
3f forms.That the rough surface of Hydroxy-Fluor-Apatite Bioceramics coating occurs is cotton-shaped, quarter butt heaped-up and the microscopic appearance such as cellular.Simulated body fluid is cultivated and is found that coatingsurface has the deposition of calcium phosphorus phase, and after SBF soaks, it is principal element apatite layer that ceramic coating surface deposition has the Ca of take, P, O, and this shows that the ceramic coating of the formation after laser melting coating has certain biological activity.Show that coating has certain biological activity.The microhardness value of ceramic layer is the highest, and maximum is 421HV
0.2.
Example 3:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=1kW, and scan velocity V=200mm/min, spot size D=15mm * 2mm, and adopt argon shield.Now, because laser power is larger, coating ripple rises and falls greatly, obviously discontinuous, and TC4 substrate ftractures, bio-ceramic coating that can not excellent.
Example 4:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=0.7kW, and scan velocity V=150mm/min, spot size D=15mm * 2mm, and adopt argon shield.Now, substrate shows to have occurred consolidation phenomenon, and reason is that sweep velocity is slower, thus too much volatilization and the vaporization of ceramic coating of unit surface absorbing laser energy, cause coating that laser melting phenomenon has occurred, do not form the fluorine-containing bio-ceramic coating combining with substrate.
Example 5:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=0.7kW, and scan velocity V=250mm/min, spot size D=15mm * 2mm, and adopt argon shield.Now, microstructure observation does not find obvious ceramic layer, and because sweep velocity is too fast, the laser energy that unit surface absorbs is relatively less, cannot fully induce coated substance generation chemical reaction, thereby fail to form ceramic coating.
Example 6:
(1) the Calcium Fluoride (Fluorspan) powder that is 1.5% by weight percent and 98.5% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt optical fiber laser to carry out circular light spot laser melting coating to the prefabricated coating on titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=1kW, and scan velocity V=720mm/min, spot size φ=6mm, and adopt argon shield.Now, most of coating glaze shape that is white in color is evenly distributed on TC4 substrate, does not occur obvious corrugated surface, and microhardness shows, the highest microhardness value 370HV of coating
0.2with substrate hardness value 360HV
0.2be more or less the same, illustrate that F content is too low and be unfavorable for forming high performance fluorine-containing bio-ceramic coating.
Example 7:
(1) the Calcium Fluoride (Fluorspan) powder that is 1.9% by weight percent and 98.1% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt optical fiber laser to carry out circular light spot laser melting coating to the prefabricated coating on titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=1kW, and scan velocity V=720mm/min, spot size φ=6mm, and adopt argon shield.Now, there is lamellar in substrate surface, and micro-metallographic shows that coating is comprised of microtextures such as class coralliform shape tissue, dendrite and particulate state; And regional area has occurred that aperture is about the micropore of l ~ 10 μ m, growth is sought connections with along implant surfaces or inside by the micropore Ke Shi freshman bone tissue being interconnected; In ceramic layer, observe micro-crack.EDS analyzes and shows, the main thing of Hydroxy-Fluor-Apatite Bioceramics coating is mutually mainly by Ti, Ti
8.86v
1.14, Al
3v, TiO
2, CaF
2, Ca
3(PO
4)
2xH
2o and Ca
5(PO
4)
3f forms, and simulated body fluid culture experiment shows, this coating has certain biological activity.
Example 8:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix; Particularly, above-mentioned powder is mixed, adopts ball mill that mixed powder is carried out ball milling refinement and evenly mixed,
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate, particularly, utilizes manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, to form preset coating, the thickness of coating is 0.3mm.
(4) adopt optical fiber laser to carry out circular light spot laser melting coating to the prefabricated coating on titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating.The processing parameter that cladding process adopts is: laser output power P=1.0kW, and scan velocity V=720mm/min, spot size φ=6mm, and adopt argon shield.Now, coating microhardness maximum reaches 1119HV
0.2, illustrate and increase within the specific limits fluorine content, be conducive to improve the microhardness of coating; Coating substance is mutually mainly by Ti, CaTiO
3, Ca
2p
2o
7, Ca
x+2p
2xo
6x+2and Ca
10(PO
4)
6(OH)
2form; Simulated body fluid culture experiment shows, coating is easy to the deposition of calcium phosphorus phase, cultivates after 7 days, and the ratio of calcium and phosphorus in coating in Ca/P ratio and skeleton is more approaching.
Following table 1 compares for the performance perameter to different embodiments of the invention:
Table 1
By thing phase composite, surface topography, biological activity and microhardness to different embodiment, contrast, can find that the resulting effect of processing parameter of embodiment 8 is better.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a method of preparing Hydroxy-Fluor-Apatite Bioceramics coating, is characterized in that, comprises the following steps:
(1) the Calcium Fluoride (Fluorspan) powder that is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix;
(2) utilizing concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3) deployed mixed powder is preset on titanium alloy substrate;
(4) adopt carbon dioxide laser to carry out broadband laser cladding to titanium alloy substrate; to generate Hydroxy-Fluor-Apatite Bioceramics coating; the processing parameter that cladding process adopts is: carbon dioxide laser laser output power P=0.5-1kW; scan velocity V=150-250mm/min; rectangular light spot dimension D=15mm * 2mm, and adopt argon shield.
2. method according to claim 1, is characterized in that, in step (1), is to adopt ball mill that mixed powder is carried out ball milling refinement and evenly mixed.
3. method according to claim 1, is characterized in that, in step (3), is to utilize manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, and to form preset coating, the thickness of coating is 0.3mm.
4. a method of preparing Hydroxy-Fluor-Apatite Bioceramics coating, is characterized in that, comprises the following steps:
The Calcium Fluoride (Fluorspan) powder that (1 ') is 2.3% by weight percent and 97.7% hydroxyapatite powder evenly mix;
(2 ') utilizes concentration is that 2% polyvinyl alcohol solution is allocated mixed powder as binding agent;
(3 ') is preset at deployed mixed powder on titanium alloy substrate;
(4 ') adopts optical fiber laser to carry out broadband laser cladding to titanium alloy substrate, to generate Hydroxy-Fluor-Apatite Bioceramics coating, the processing parameter that cladding process adopts is: optical fiber laser laser power 0.8-1kw, sweep velocity 720mm/min, tabula rasa size
and adopt argon shield.
5. method according to claim 4, is characterized in that, in step (1 '), is to adopt ball mill that mixed powder is carried out ball milling refinement and evenly mixed.
6. method according to claim 4, is characterized in that, in step (3 '), is to utilize manual spray gun and air compressor mixed powder to be sprayed on to the surface of titanium alloy substrate, and to form preset coating, the thickness of coating is 0.3mm.
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| CN103981519B (en) * | 2014-05-30 | 2017-01-11 | 山东大学 | Method for laser cladding of wollastonite-based bioactive ceramic coating on surface of titanium alloy |
| CN105018924B (en) * | 2014-11-14 | 2017-12-26 | 中国兵器工业第五二研究所 | A kind of preparation method of titanium alloy substrate hydroxyapatite coating on surface |
| CN105293462A (en) * | 2015-12-02 | 2016-02-03 | 杭州电子科技大学 | Method of preparing hydroxyapatite by mechanochemical method |
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