CN104042350A - Implant with plasma coated nano-zirconium oxide coating and preparation method thereof - Google Patents
Implant with plasma coated nano-zirconium oxide coating and preparation method thereof Download PDFInfo
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- CN104042350A CN104042350A CN201410294481.1A CN201410294481A CN104042350A CN 104042350 A CN104042350 A CN 104042350A CN 201410294481 A CN201410294481 A CN 201410294481A CN 104042350 A CN104042350 A CN 104042350A
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Abstract
The invention relates to an implant with a plasma coated nano-zirconium oxide coating and a preparation method thereof. The implant comprises an implant body and an abutment, wherein the implant body is conical and is provided with threads; the abutment comprises a gum penetrating part, a shoulder and an abutment part; the gum penetrating part is conical and is fixedly connected with the implant body; the abutment part is conical and is fixedly connected with the gum penetrating part by virtue of the shoulder. The implant is made from a pure titanium or titanium alloy material, and is of a one-piece integral structure; the surfaces of the gum penetrating part and the shoulder are uniformly coated with a nano-zirconium oxide coating. The preparation method is performed in a mode of finely cutting and coating with plasma. The implant is made from a pure titanium or titanium alloy material and is of a one-piece integral structure, and the nano-zirconium oxide coating is uniformly coated to the surfaces of the gum penetrating part and the shoulder; the implant has the nice appearance of the zironium oxide abutment and excellent bioavailability, and has the mechanical strength of a titanium abutment.
Description
Technical field
The present invention relates to a kind of implantation body and preparation method thereof, relate in particular to implantation body of a kind of pure titanium or the nano oxidized zirconium coating of titanium alloy surface plasma spraying and preparation method thereof, belong to Dental Implant material technology field.
Background technology
Along with stomatologic development, it is ripe that Dental Implant technology has been tending towards, and implantation body is the topmost instrument of using in Dental Implant process.Implantation body generally comprises implantation body's body and base station, and base station is the important structure that connects implantation body's body and upper prosthesis, and it and soft tissue, dummy and patient's oral environment around jointly successfully maintain and play an important role implant denture.At present the pure titanium or titanium alloy base station of application has good biocompatibility clinically, can be good at rubbing and joining pair with implantation body body; But Tai Lei base station implantation body shoulder position is higher, in the thinner patient of labial teeth district gingiva, can exposing metal color and affect attractive in appearance.Zirconium oxide base station has good biocompatibility and aesthetic properties, more can meet the demand of clinical repair treatment; But its intensity is lower, fragility is higher and easy jackknifing breaks.Therefore, for problems such as the poor and zirconium oxide base station bad mechanical properties of titanium class base station aesthetic property, research and develop a kind of aesthetic property and good biocompatibility of existing zirconium oxide base station, have again the novel base station of the mechanical strength of titanium class base station, there is higher clinical value and wide market prospect.
Chinese patent literature CN101972174A discloses dental implantation prosthesis and the manufacture method that a kind of ZrO2-HA is compound, it is characterized in that described implant prosthesis is one-part form implant prosthesis, it is taking ZrO2 pottery as matrix, the implant prosthesis being mechanically connected with HA, described implant prosthesis fills position by top, cervical region, shoulder, HA successively and screw-like head forms.Described implant prosthesis is cylinder, cylindrical symmetrical both sides, top.Top to shoulder is smooth curve, to ensure that gingival epithelium has well and conforms to implant prosthesis under least energy.It is regular hole that HA fills position, is positioned at the following 0.5-1mm of shoulder.But this implant prosthesis is taking zirconium oxide as matrix, intensity is lower, fragility is higher and easy jackknifing breaks.
Summary of the invention
For the deficiencies in the prior art, the invention provides implantation body of the nano oxidized zirconium coating of a kind of plasma spraying and preparation method thereof.
Technical scheme of the present invention is as follows:
An implantation body for the nano oxidized zirconium coating of plasma spraying, comprises implantation body's body and base station, and described implantation body's body is tapered and be provided with screw thread; Described base station comprises wears gum portion, shoulder and abutment portion, wears gum portion tapered and be fixedly connected with implantation body body, described abutment portion tapered and by shoulder with wear gum portion and be fixedly connected with; This implantation body is pure titanium or titanium alloy material and is one-part form overall structure, and the described surface uniform of wearing gum portion and shoulder is coated with nano oxidized zirconium coating.
According to the present invention, preferred, the thickness of described nano oxidized zirconium coating is 100-500 μ m, more preferably 300-400 μ m.
According to the present invention, preferred, the long 12-16mm of described implantation body.
According to the present invention, preferred, the described long 5-8mm of implantation body's body, maximum gauge is 4-6mm.
According to the present invention, preferred, the described gum minister 2-4mm that wears, the diameter of shoulder is 6-8mm, base station minister 2-4mm.
According to the present invention, preferred, extend to and within the scope of abutment portion 1mm, be also evenly coated with nano oxidized zirconium coating from shoulder.
According to the present invention, the preparation method of the implantation body of the nano oxidized zirconium coating of above-mentioned plasma spraying, step is as follows:
(1) by after medical pure titanium rod or titanium alloy bar cutting, adopt meticulous lathe machine cut to become one-part form implantation body;
(2) implantation body is soaked to 5-8min with alkali at 60-80 DEG C, after being cooled to room temperature, use distilled water flushing 5-8min, be placed in acetone ultrasonic irrigation 10-15min, then be placed in ethyl ketone ultrasonic irrigation 10-15min, finally use distilled water flushing three times, every all over 10-15min;
(3) will carry out blasting treatment through step (2) implant surface after treatment;
(4) gum portion is being worn to and shoulder surface plasma sprays nano oxidized zirconium coating by the implantation body after step (3) blasting treatment, concrete steps are:
The nano zircite pelletizing that is 70～110nm with particle diameter, as raw material, is agglomerated into spherical or oval-shaped spherical powder by pelletizing, crosses 325～400 mesh sieves;
To wear gum portion and shoulder surface spraying nano zircite pelletizing, spray parameters: arc voltage 80-85V, arc current 450-550A, primary air amount 2.0-2.5m
3h
-1, secondary streams amount 1.0-1.5m
3h
-1, carrier gas flux 0.3-0.5m
3h
-1, powder feed rate 35-45g/min, spray distance 65-75mm;
(5) sprayed the rear oxirane disinfection of using, to have obtained final product.
According to the present invention, preferred, the pure titanium rod described in step (1) or the long 7cm of titanium alloy bar, diameter 8mm.
According to the present invention, preferred, the alkali described in step (2) is the sodium hydroxide solution of concentration 20-40wt%.
According to the present invention, preferred, in step (4), nano zircite pelletizing is stabilized with yttrium oxide type four directions nano zircite pelletizing; Extend to and within the scope of abutment portion 1mm, be also evenly coated with nano oxidized zirconium coating from shoulder.
According to the present invention, preferred, the spray parameters described in step (4): arc voltage 82V, arc current 500A, primary air amount 2.1m
3h
-1, secondary streams amount 1.3m
3h
-1, carrier gas flux 0.4m
3h
-1, powder feed rate 40g/min, spray distance 70mm.
Beneficial effect of the present invention:
1, the implantation body of the nano oxidized zirconium coating of plasma spraying of the present invention is pure titanium or titanium alloy material and is one-part form overall structure, is coated with nano oxidized zirconium coating at the surface uniform of wearing gum portion and shoulder; So not only there are aesthetic property and the good biocompatibility of zirconia base platform, have again the mechanical strength of titanium class base station.
2, the adhesion strength of the nano oxidized zirconium coating of the present invention is high, and the implantation body of preparation has good cell compatibility.
3, the preparation method of the implantation body of the nano oxidized zirconium coating of plasma spray of the present invention is simple, adopts plasma spray coating process spraying, and not only than calcine technology energy efficient, and the adhesion strength of nano oxidized zirconium coating is high.
Brief description of the drawings
Fig. 1 is the structural representation that the present invention sprays the implantation body of nano oxidized zirconium coating.
Fig. 2-6 are the stretched test rear oxidation of the test specimen zirconium nano coating of different nano zircite coating layer thicknesses in experimental example 2 of the present invention and the SEM of titanio bottom interface figure.
Wherein, 1, implantation body's body, 2, base station, 2-1, wear gum portion, 2-2, shoulder, 2-3, abutment portion.
Detailed description of the invention
Below by specific embodiment, also the present invention will be further described by reference to the accompanying drawings, but be not limited to this.
Embodiment 1
An implantation body for the nano oxidized zirconium coating of plasma spraying, this implantation body is pure titanium material and for one-part form overall structure, comprises implantation body's body 1 and base station 2, described implantation body's body 1 is tapered and be provided with screw thread; Described base station 2 comprises wears the 2-1 of gum portion, shoulder 2-2 and abutment portion 2-3, wears the 2-1 of gum portion tapered and be fixedly connected with implantation body body 1, described abutment portion 2-3 tapered and by shoulder 2-2 with wear the 2-1 of gum portion and be fixedly connected with; The described surface uniform of wearing the 2-1 of gum portion and shoulder 2-2 is coated with nano oxidized zirconium coating; Extend to from shoulder 2-2 within the scope of the 1mm of abutment portion 2-3 and be also evenly coated with nano oxidized zirconium coating.
In the present embodiment, the thickness of nano oxidized zirconium coating is 100 μ m, the long 13.5mm of implantation body; The long 7mm of implantation body's body 1, maximum gauge is 6mm; Wear the long 3mm of the 2-1 of gum portion; The diameter of shoulder 2-2 is 7mm; The long 3.5mm of abutment portion 2-3.
The preparation method of the implantation body of the nano oxidized zirconium coating of the present embodiment plasma spraying, step is as follows:
(1) will long 7cm, after the medical pure titanium rod cutting that diameter is 8mm, adopt meticulous lathe machine cut to become one-part form implantation body;
(2) sodium hydroxide solution that is 30wt% by implantation body by concentration soaks 5min at 60 DEG C, after being cooled to room temperature, use distilled water flushing 5min, be placed in acetone ultrasonic irrigation 10min, then be placed in ethyl ketone ultrasonic irrigation 10min, finally use distilled water flushing three times, every all over 10min;
(3) will be through 16# corundum sand blasting treatment for step (2) implant surface after treatment;
(4) 2-1 of gum portion is being worn to and shoulder 2-2 surface plasma sprays nano oxidized zirconium coating in the implantation body after step (3) blasting treatment, extending to from shoulder 2-2 within the scope of the 1mm of abutment portion 2-3 and be also evenly coated with nano oxidized zirconium coating;
Concrete steps are:
The stabilized with yttrium oxide type that is 70nm with particle diameter four directions nano zircite pelletizing, as raw material, is agglomerated into spherical or oval-shaped spherical powder by pelletizing, crosses 325 mesh standard sieves; Adopt the high energy plasma spray gun that nozzle diameter is 6.5mm to move back and forth, spray gun translational speed is set as 600mm/s, and coating is painted on and wears the 2-1 of gum portion and shoulder 2-2 surface;
Spray parameters: arc voltage 82V, arc current 500A, primary air amount 2.1m
3h
-1, secondary streams amount 1.3m
3h
-1, carrier gas flux 0.4m
3h
-1, powder feed rate 40g/min, spray distance 70mm;
(5) sprayed the rear oxirane disinfection of using, to have obtained final product.
Embodiment 2
The implantation body of the nano oxidized zirconium coating of plasma spraying as described in Example 1, different is that implantation body is titanium alloy material; The thickness of nano oxidized zirconium coating is 300 μ m, the long 12mm of implantation body; The long 5mm of implantation body's body 1, maximum gauge is 4mm; Wear the long 3mm of the 2-1 of gum portion; The diameter of shoulder 2-2 is 6mm; The long 4mm of abutment portion 2-3.
The preparation method of the implantation body of the nano oxidized zirconium coating of plasma spraying is with embodiment 1, different:
The sodium hydroxide solution that is 35wt% by concentration in step (2) soaks 8min at 80 DEG C, after being cooled to room temperature, use distilled water flushing 8min, be placed in acetone ultrasonic irrigation 15min, then be placed in ethyl ketone ultrasonic irrigation 15min, finally use distilled water flushing three times, every all over 15min;
Spray parameters in step (4): arc voltage 85V, arc current 550A, primary air amount 2.5m
3h
-1, secondary streams amount 1.5m
3h
-1, carrier gas flux 0.5m
3h
-1, powder feed rate 45g/min, spray distance 75mm.
Embodiment 3
The implantation body of the nano oxidized zirconium coating of plasma spraying as described in Example 1, different is that implantation body is pure titanium material; The thickness of nano oxidized zirconium coating is 500 μ m, the long 16mm of implantation body; The long 8mm of implantation body's body 1, maximum gauge is 4mm; Wear the long 4mm of the 2-1 of gum portion; The diameter of shoulder 2-2 is 6mm; The long 4mm of abutment portion 2-3.
The preparation method of the implantation body of the nano oxidized zirconium coating of plasma spraying is with embodiment 1, different:
The sodium hydroxide solution that is 40wt% by concentration in step (2) soaks 6min at 70 DEG C, after being cooled to room temperature, use distilled water flushing 6min, be placed in acetone ultrasonic irrigation 12min, then be placed in ethyl ketone ultrasonic irrigation 12min, finally use distilled water flushing three times, every all over 12min;
Spray parameters in step (4): arc voltage 80V, arc current 450A, primary air amount 2.0m
3h
-1, secondary streams amount 1.0m
3h
-1, carrier gas flux 0.3m
3h
-1, powder feed rate 35g/min, spray distance 65mm.
Experimental example 1 biocompatibility detects
By the series standard requirement in ISO10993.12-2009 and national GB/T16886-2008, the implantation body of the nano oxidized zirconium coating of plasma spraying prepared by embodiment 1 carries out hemolytic experiment, cytotoxicity experiment, Wistar subcutaneous rat implantation experiment, with its biocompatibility of overall merit.
(1) the diluted fresh anticoagulant Sanguis Leporis seu oryctolagi of hemolytic experiment: 0.2ml and 10ml0.9%NS (negative control group and experimental group), 10ml distilled water (positive controls) add respectively centrifuge tube, in experimental group, add base station test specimen, centrifugal and detect the absorbance of each sample supernatant after water-bath, find that experimental group does not cause external hemolytic reaction.
(2) cytotoxicity experiment: with three groups of culture fluid (implantation body's lixiviating solution of the nano oxidized zirconium coating of plasma spraying, the culture fluid containing 6.4% phenol, normal culture fluid) cultivation Mouse L929 cell, discovery cell attachment is good, cell is fusiformis, cell is prominent fully to be stretched, and refractivity is strong.Adjusting cell concentration is that 5 × 104/mL is inoculated in 96 orifice plates, the relative rate of increase (RGR) that adopts CCK-8 method to record L929 cell culture 24h, 48h, 72h is respectively 97.3%, 96.5% and 96.3%, no cytotoxicity, reaction is I level, and this result shows that there is good cell compatibility in the implantation body of the nano oxidized zirconium coating of plasma spraying.
(3) subcutaneous rat is implanted experiment: 24 of clean level Wistar rats, random packet.Rat back spinal column left and right side is prepared leather bag and is implanted implantation body and the pure titanio platform of the nano oxidized zirconium coating of sterilizing plasma spraying, and right side is as experimental group, and left side as a control group.Implant and initially cause that material surrounding tissue mild inflammation reacts, see that inflammatory cell is dispersed in infiltration, inflammatory reaction alleviates after 1 week, has fibrous capsule formation but comparatively loose.After 2 weeks, in the Peri-implant tissues of the visible nano oxidized zirconium coating of plasma spraying, have neutrophilic granulocyte and lymphocytic infiltration, quantity reduces, and fibrous capsule thickens.After 4 weeks, in the Peri-implant tissues of the nano oxidized zirconium coating of observation plasma spraying, still have a small amount of lymphocyte, neutrophilic granulocyte, the hyperemia of skin corium inner tissue alleviates, and a large amount of collagen fiber of bone regeneration around implant of the nano oxidized zirconium coating of plasma spraying form comparatively fine and close fibrous capsule; Implant fibrous capsule attenuation gradually after 8 weeks, 12 weeks, in implant surrounding tissue, inflammatory reaction disappears substantially.
Experimental example 2 anchoring strength of coating tests
Prepare 65 of the long pure titanium rods (diameter 8mm) of 7 ㎝, choose at random 35 and make spraying test specimen, be divided into 5 groups, remaining 30 is test specimen to be measured (pull test is used).Adopt powder to inject plasma spraying technology and prepare respectively the nano oxidized zirconium coating that thickness is 100 μ m, 200 μ m, 300 μ m, 400 μ m and 500 μ m on the transverse section of spraying test specimen, use the microstructure of S-3700N scanning electron microscopic observation analytical pure titanium-nano zircite coating interface, to after spraying test specimen and test specimen adhesive solidification to be measured, utilize digital display electronic tensile testing machine to carry out coating pulling experiment with E-7 glue, loading force value when recording coating and stripping off, and by the microhardness of digital display microhardness testers testing coating.
(1) the tension test test result of nano oxidized zirconium coating and titanio body (unit: MPa) is as shown in table 1:
Table 1
Note: identical * count order represents two groups of there was no significant differences, different * count orders represent that two groups have significant difference (P < 0.05).
One factor analysis of variance shows P < 0.01, between explanation group, there are differences.The demonstration of LSD-t inspection statistics Epidemiological Analysis, 400 μ m group bond strength maximums, are obviously greater than other four groups (P < 0.05); 300 μ m group bond strengths are taken second place, and are obviously greater than 100 μ m groups, 200 μ m groups and 500 μ m groups (P < 0.05); 100 μ m group bond strength minimums, are significantly less than other four groups (P < 0.05).
(2) coating and matrix material morphology observation after tension test
After tension test, the SEM shape appearance figure of five groups of test specimen zirconium oxide nano coatings and titanio bottom interface is as shown in Fig. 2-6, and from Fig. 2-6, the interface at the bottom of 100 μ m coating groups and titanio has micro-crack to exist, and has a small amount of cavity to exist in coating; It is poor that the interface oxidation zirconium granule of 200 μ m groups melts degree, is coated with the visible hidden crackle of interlayer; It is better that the granule of 300 μ m groups and 500 μ m group interface melts degree, and oxide is less; Thawing degree and the flattening degree of 400 μ m coating groups are better, relatively even compact, and substantially there is not hole in coating inside.
(3) micro-hardness testing result, as shown in table 2:
Table 2
Note: identical * count order represents two groups of there was no significant differences, different * count orders represent that two groups have significant difference (P < 0.05).
The microhardness value of experiment gained zirconium oxide nano coating is between 630.96～668.14HV.The microhardness value of 300 μ m～500 μ m groups is more approaching, and discreteness is less, and the coating even compact within the scope of this is described.
Claims (10)
1. an implantation body for the nano oxidized zirconium coating of plasma spraying, is characterized in that, this implantation body comprises implantation body's body and base station, and described implantation body's body is tapered and be provided with screw thread; Described base station comprises wears gum portion, shoulder and abutment portion, wears gum portion tapered and be fixedly connected with implantation body body, described abutment portion tapered and by shoulder with wear gum portion and be fixedly connected with; This implantation body is pure titanium or titanium alloy material and is one-part form overall structure, and the described surface uniform of wearing gum portion and shoulder is coated with nano oxidized zirconium coating.
2. the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 1, is characterized in that, the thickness of described nano oxidized zirconium coating is 100-500 μ m, more preferably 300-400 μ m.
3. the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 1, is characterized in that, the long 12-16mm of described implantation body; The described long 5-8mm of implantation body's body, maximum gauge is 4-6mm.
4. the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 1, is characterized in that, the described gum minister 2-4mm that wears, and the diameter of shoulder is 6-8mm, base station minister 2-4mm.
5. the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 1, is characterized in that, extends to and within the scope of abutment portion 1mm, is also evenly coated with nano oxidized zirconium coating from shoulder.
6. a preparation method for the implantation body of the nano oxidized zirconium coating of plasma spraying claimed in claim 1, step is as follows:
(1) by after medical pure titanium rod or titanium alloy bar cutting, adopt meticulous lathe machine cut to become one-part form implantation body;
(2) implantation body is soaked to 5-8min with alkali at 60-80 DEG C, after being cooled to room temperature, use distilled water flushing 5-8min, be placed in acetone ultrasonic irrigation 10-15min, then be placed in ethyl ketone ultrasonic irrigation 10-15min, finally use distilled water flushing three times, every all over 10-15min;
(3) will carry out blasting treatment through step (2) implant surface after treatment;
(4) gum portion is being worn to and shoulder surface plasma sprays nano oxidized zirconium coating by the implantation body after step (3) blasting treatment, concrete steps are:
The nano zircite pelletizing that is 70～110nm with particle diameter, as raw material, is agglomerated into spherical or oval-shaped spherical powder by pelletizing, crosses 325～400 mesh sieves;
To wear gum portion and shoulder surface spraying nano zircite pelletizing, spray parameters: arc voltage 80-85V, arc current 450-550A, primary air amount 2.0-2.5m
3h
-1, secondary streams amount 1.0-1.5m
3h
-1, carrier gas flux 0.3-0.5m
3h
-1, powder feed rate 35-45g/min, spray distance 65-75mm;
(5) sprayed the rear oxirane disinfection of using, to have obtained final product.
7. the preparation method of the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 6, is characterized in that, the pure titanium rod described in step (1) or the long 7cm of titanium alloy bar, diameter 8mm.
8. the preparation method of the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 6, is characterized in that, the alkali described in step (2) is the sodium hydroxide solution of concentration 20-40wt%.
9. the preparation method of the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 6, is characterized in that, in step (4), nano zircite pelletizing is stabilized with yttrium oxide type four directions nano zircite pelletizing; Extend to and within the scope of abutment portion 1mm, be also evenly coated with nano oxidized zirconium coating from shoulder.
10. the preparation method of the implantation body of the nano oxidized zirconium coating of plasma spraying according to claim 6, is characterized in that, the spray parameters described in step (4): arc voltage 82V, arc current 500A, primary air amount 2.1m
3h
-1, secondary streams amount 1.3m
3h
-1, carrier gas flux 0.4m
3h
-1, powder feed rate 40g/min, spray distance 70mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420662A (en) * | 2015-12-09 | 2016-03-23 | 山东大学 | Method for spraying nano-zirconia coating onto pure-titanium surface through plasma spraying suitable for synosteosis |
| CN108272520A (en) * | 2018-02-12 | 2018-07-13 | 佛山科学技术学院 | A kind of integral type plantation base station |
-
2014
- 2014-06-25 CN CN201410294481.1A patent/CN104042350A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420662A (en) * | 2015-12-09 | 2016-03-23 | 山东大学 | Method for spraying nano-zirconia coating onto pure-titanium surface through plasma spraying suitable for synosteosis |
| CN105420662B (en) * | 2015-12-09 | 2018-01-23 | 山东大学 | A kind of method that pure titanium surface plasma for being easy to synosteosis sprays nanostructured zirconia coating |
| CN108272520A (en) * | 2018-02-12 | 2018-07-13 | 佛山科学技术学院 | A kind of integral type plantation base station |
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