CN118580067A - Surface treatment method of zirconium oxide implant and its application - Google Patents
Surface treatment method of zirconium oxide implant and its application Download PDFInfo
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Abstract
本发明提供了一种氧化锆种植体的表面处理方法及其应用。本发明的表面处理方法具体包括：(1)将种植体的原料充填到模具的金属模腔内，经压制成型、一次烧结后，得到坯体；(2)表面喷砂和酸蚀处理：对步骤(1)得到的坯体的表面依次进行喷砂处理和酸蚀处理，随后再进行终烧结，得到所述种植体。通过本发明的表面处理方法不仅可以制备得到具有宏观形貌和微观形貌的种植体，得到的种植体的成分基本与原料相同，且杂质含量更少，不会造成表面成分的改变，从而维持较好的材料性能。
The present invention provides a surface treatment method for a zirconia implant and its application. The surface treatment method of the present invention specifically comprises: (1) filling the raw material of the implant into the metal mold cavity of the mold, and obtaining a blank after compression molding and primary sintering; (2) surface sandblasting and acid etching treatment: the surface of the blank obtained in step (1) is sequentially sandblasted and acid-etched, and then finally sintered to obtain the implant. The surface treatment method of the present invention can not only prepare an implant with macroscopic and microscopic morphology, but also the composition of the obtained implant is basically the same as the raw material, and the impurity content is less, which will not cause changes in the surface composition, thereby maintaining good material properties.
Description
Technical Field
The invention relates to the technical field of medical biological implant materials, in particular to a surface treatment method of a zirconia implant, and particularly relates to a method for preparing a surface morphology beneficial to bone union on the surface of the zirconia implant.
Background
The dental implant technology is a technology for replacing artificial teeth to perform functions after dentition defect or missing. The biological basis for the function of an implant is the theory of osseointegration. That is, under an optical microscope, bone tissue is directly combined with the surface of the loadable implant without fibrous tissue intervention. The osseointegration is in dynamic balance and stable for a long time.
At present, the implant materials commonly used are pure titanium (TA 4) or titanium alloy (Ti-6 Al-4V, TC4 and Ti-Zr), and the metals or the metal alloys have good mechanical strength and good osseointegration performance and can bear chewing pressure well. However, the metal material has inherent defects such as local allergy and local enrichment after metal ions are dissolved out, higher electric conductivity and thermal conductivity damage periodontal tissues, peri-implant inflammation caused by metal particles, easy adhesion of metal plaque and the like, especially black gray metal color, and the penetration part often has a penetration green and a neck margin grey line, which affect the appearance.
In order to solve these problems, zirconia materials are becoming suitable alternative materials, zirconia itself has excellent mechanical strength and biocompatibility, is a poor conductor of electricity and heat, does not generate micro-current and thermal burn, and is not caused to be inflamed or allergic by immune system as foreign matters due to ion elution, in particular, its beautiful color, so that it is suitable to be placed at aesthetic sites.
Artificial materials are typically surface treated so that the material is more easily bonded to bone with a higher rate of bonding. For metal materials, there are methods such as sand blasting, acid etching, laser, surface coating, surface building structure, ultraviolet light, etc. For ceramics, the ceramics have the defects of high hardness, difficult reaction with materials and the like, and are difficult to process.
Disclosure of Invention
In order to solve the technical problems, the invention provides a surface treatment method of a zirconia implant, which does not damage the surface structure of a material and can form good osseointegration.
The technical scheme of the invention is as follows:
the surface treatment method of the zirconia implant specifically comprises the following steps:
(1) Filling raw materials of the implant into a metal die cavity of a die, and obtaining a blank after press forming and primary sintering;
(2) Surface blasting and acid etching treatment: and (3) sequentially carrying out sand blasting treatment and acid etching treatment on the surface of the green body obtained in the step (1), and then carrying out final sintering to obtain the implant.
According to an embodiment of the present invention, in step (1), the raw materials of the implant include at least:
5 to 5.5 weight percent of yttrium oxide,
The hafnium oxide is not more than 5wt%,
88-95% Of zirconia.
Further, the raw material of the implant further includes impurities known in the art, and the content of the impurities is not more than 1wt%.
According to an embodiment of the invention, the specific surface area of the raw material of the implant is 10-50m 2/g, for example 20m 2/g.
According to an embodiment of the invention, the raw material of the implant is a powder having a particle size of 0.01-0.1 μm, for example 0.04 μm.
Illustratively, the raw material of the implant has a particle size of 0.04 μm and a specific surface area of 20m 2/g.
According to an embodiment of the present invention, in step (1), the press forming may be performed by methods known in the art, such as dry press forming or isostatic press forming. Illustratively, the press forming is isostatic forming at 450 MPa.
According to an embodiment of the present invention, in step (1), the mold may be selected from molds known in the art, and may be prepared using, for example, a metal material selected from, but not limited to, at least one of stainless steel, aluminum alloy, titanium alloy, and the like.
According to an embodiment of the present invention, in step (1), the conditions of the primary sintering are: pressureless sintering is carried out at 900-1100 ℃ for 2-8 hours. Preferably, the temperature rising rate is 2-5 ℃/min before the primary sintering. Preferably, after primary sintering, naturally cooling to obtain a green body.
According to an embodiment of the invention, the blasting treatment comprises blasting sand balls onto the surface of the blank. Preferably, the sand spheres are selected from boron carbide, zirconia or alumina, preferably zirconia, more preferably alumina. Preferably, the sand spheres have a diameter of 50-500 μm, preferably 80-400 μm, more preferably 100-200 μm. Further, the sandblasting pressure is 1-10bar, for example 2-5bar; the working distance of the blasting is 10-50mm, for example 15mm, preferably 8-10mm; the moving speed of the blasting is 1-20mm/s, for example 5mm/s.
According to an embodiment of the present invention, in step (2), the etching process includes: the surface of the green body is treated by etching liquid, and substances which are easy to remove in the green body, such as alkaline or amphoteric oxides of calcium phosphate, calcium oxide, magnesium oxide and the like, are removed without affecting the performance of a raw material matrix (such as zirconium oxide) in the implant.
According to an embodiment of the present invention, the etching solution includes a first acid and hydrofluoric acid. Preferably, the first acid may be selected from at least one, two or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and the like. Further, the hydrofluoric acid is selected from 30-50vol% hydrofluoric acid; the first acid is selected from 50-80vol% nitric acid or 30-50vol% sulfuric acid, 40-60vol% phosphoric acid. More preferably, the etching solution is obtained by mixing 30 to 50vol% hydrofluoric acid with 50 to 80vol% nitric acid, preferably 35 to 45vol% hydrofluoric acid with 60 to 70vol% nitric acid. Illustratively, the etching solution includes hydrofluoric acid (40 vol%) and nitric acid (50 vol%) in a volume ratio of 4:6.
According to an embodiment of the present invention, in the etching solution, the volume ratio of the hydrofluoric acid to the first acid is (2-8): (8-2), preferably (4-6): (6-4), more preferably 4:6.
Preferably, the etching time is 1min to 120min, preferably 20min to 40min, more preferably 30min.
Preferably, the temperature of the etching is 30-100 ℃, for example 70 ℃, 80 ℃.
According to an embodiment of the present invention, in step (2), the final sintering includes: sintering temperatures are 1450-1530 ℃, for example 1500 ℃; the sintering time is 1.5h-2.5h, for example 2h.
According to an embodiment of the present invention, cleaning may also be performed after the blasting, acid etching or final sintering. Preferably, the cleaning comprises: washing with sodium chloride solution or deionized water, which may be performed by methods known in the art, such as by ultrasonic vibration; preferably, the time of the washing is 1 to 10 minutes.
The invention also provides a surface topography of an implant, which is prepared by the surface treatment method.
According to an embodiment of the present invention, the raw materials of the implant include at least:
5 to 5.5 weight percent of yttrium oxide,
The hafnium oxide is not more than 5wt%,
88-95% Of zirconia.
Further, the raw material of the implant further includes impurities known in the art, and the content of the impurities is not more than 1wt%.
According to an embodiment of the invention, the surface of the implant has a roughness Ra of 1-5 μm, for example 1.6 μm, 1.8 μm, 2.4 μm.
The invention also provides an implant, and the surface of the implant comprises the surface morphology of the implant.
According to an embodiment of the present invention, the raw materials of the implant include at least:
5 to 5.5 weight percent of yttrium oxide,
The hafnium oxide is not more than 5wt%,
88-95% Of zirconia.
Further, the raw material of the implant further includes impurities known in the art, and the content of the impurities is not more than 1wt%.
According to an embodiment of the invention, the surface of the implant has a roughness Ra of 1-5 μm, for example 1.6 μm, 1.8 μm, 2.4 μm.
The invention also provides an implant, the surface of which is prepared by the surface treatment method.
According to an embodiment of the present invention, the raw materials of the implant include at least:
5 to 5.5 weight percent of yttrium oxide,
The hafnium oxide is not more than 5wt%,
88-95% Of zirconia.
Further, the raw material of the implant further includes impurities known in the art, and the content of the impurities is not more than 1wt%.
According to an embodiment of the invention, the surface of the implant has a roughness Ra of 1-5 μm, for example 1.6 μm, 1.8 μm, 2.4 μm.
The invention also provides application of the implant in medical biological implant materials.
Advantageous effects
The invention provides a surface treatment method of an implant, which can be used for preparing the implant with macroscopic morphology and microscopic morphology, the components of the obtained implant are basically the same as the raw materials, the impurity content is less, the change of the surface components is not caused, and thus, the better material performance is maintained.
Drawings
Fig. 1 is an electron microscopic view of the zirconia material of example 1.
FIG. 2 is a scale of alkaline phosphatase (ALP) staining and semi-quantitative analysis of example 3: 200 μm.
FIG. 3 shows the results of the CCK8 assay of example 4 for BMSCs proliferation activity.
Detailed Description
The technical scheme of the invention will be further described in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
Example 1
The surface treatment method of the zirconia material comprises the following steps:
1. Selecting zirconia powder with the grain diameter of 0.04 mu m and the specific surface area of 20m 2/g, filling the zirconia powder into a mould, carrying out dry pressing forming, carrying out isostatic pressing under 450MPa, pressing into a biscuit, carrying out pressureless sintering at 1100 ℃, keeping the temperature for 5 hours, and naturally cooling at the heating rate of 5 ℃/min to obtain a sintered zirconia bar;
2. adopting alumina particles with the diameter of 200 mu m, wherein 15mm is arranged between a nozzle and the sintered zirconia bar in the step 1, the moving speed is 5mm/s, and the sand blasting pressure is 2bar;
3. After the sand blasting, washing the zirconia bar after the sand blasting by deionized water;
4. preparing an etching solution: mixing 40vol% of hydrofluoric acid and 50vol% of nitric acid according to a volume ratio of 4:6 to obtain etching solution;
5. Etching the surface of the zirconia rod obtained in the step 3 by adopting the etching solution in the step 4, wherein the etching time is 30min, and the temperature is 80 ℃; ultrasonically cleaning with deionized water for 5min after etching;
6. final sintering is carried out on the treated zirconia material, wherein the sintering conditions comprise: the sintering temperature is 1500 ℃, and the sintering time is 2 hours; a suitable surface topography is obtained as shown in fig. 1.
Example 2
The zirconia material prepared in example 1 was taken and subjected to surface roughness test. The roughness of the zirconia material is 1.6 mu m, which is suitable for the growth of osteoblasts.
Example 3
1. Osteoblast performance test of cells on the surface of the material:
A zirconia disk having a diameter of 14mm was prepared with reference to example 1, except that: in the step 1, the selected moulds are different, and the zirconia disc with phi of 14mm is finally prepared; the rest of the procedure was as in example 1, finally obtaining zirconia discs with a surface roughness of 1.6 μm and a diameter of 14mm.
2. The zirconia disc was placed on the bottom of a 24-well plate after being washed and sterilized, and cell culture and osteogenesis were performed, and a pure titanium sample was used as a control group.
The specific steps of cell culture and osteogenesis assay are as follows:
(1) The well-conditioned P3 BMSCs were inoculated into 24-well plates at a density of 1X 10 4cells/cm2, 1.5ml of an alpha-MEM medium containing 1% of diabody (green streptomycin, commercially available) and 10% of FBS was added, and the mixture was placed in an incubator at 37℃and 5% CO 2 for culturing, and the medium was changed 1 time every 2 days.
(2) When the cell growth is converged to 60%, the original culture medium is removed, PBS is washed for 2 times, and 1.5ml of osteogenesis induction culture solution is added; the culture was continued for 10 days with 1 exchange of the liquid every 3 days.
(3) ALP staining and semi-quantitative analysis were performed on BMSCs that had undergone osteoinduction according to the finished ALP staining kit method. The results are shown in FIG. 2, where the scale is 200. Mu.m.
As can be seen from FIG. 2, both the zirconia disc and the pure titanium disc showed positive ALP staining, and the two were semi-quantitatively analyzed without statistical difference, thereby proving that the zirconia treated by the surface treatment method of the present invention can be well osteogenic.
Example 4
Proliferation ability of cells on implant surface:
Referring to example 3, a zirconium oxide disc of phi 14mm was prepared, washed and sterilized, then placed in a 24-well plate, cell culture was performed, surface cell proliferation of the zirconium oxide disc was analyzed using CCK8 kit, and pure titanium implant was used as a control group. The cell proliferation assay specifically includes: BMSCs were cultured on the surfaces of zirconia discs and pure titanium implants for 1-8 days, respectively, and BMSCs proliferation activity was examined by CCK8 method. The test results are shown in FIG. 3.
As can be seen from FIG. 3, the proliferation of cells on the surface of the zirconia disk increased logarithmically, similar to that of the control group, indicating that the zirconia disk treated by the surface treatment method of the present invention had a proliferation reaction similar to that of pure titanium.
The above description of exemplary embodiments of the application has been provided. The scope of the application is not limited to the embodiments described above. Any modifications, equivalent substitutions, improvements, or the like, which are within the spirit and principles of the present application, should be made by those skilled in the art, and are intended to be included within the scope of the present application.
Claims (10)
1. The surface treatment method of the zirconia implant is characterized by comprising the following steps:
(1) Filling raw materials of the implant into a metal die cavity of a die, and obtaining a blank after press forming and primary sintering;
(2) Surface blasting and acid etching treatment: and (3) sequentially carrying out sand blasting treatment and acid etching treatment on the surface of the green body obtained in the step (1), and then carrying out final sintering to obtain the implant.
2. The surface treatment method according to claim 1, wherein in the step (1), the raw materials of the implant include at least:
5 to 5.5 weight percent of yttrium oxide,
The hafnium oxide is not more than 5wt%,
88-95% Of zirconia.
Preferably, the specific surface area of the raw material of the implant is 10-50m 2/g.
Preferably, the raw material of the implant is powder, and the particle size of the powder is 0.01-0.1 mu m.
3. The surface treatment method according to claim 1, wherein in the step (1), the condition of the primary sintering is: pressureless sintering is carried out at 900-1100 ℃ for 2-8 hours. Preferably, the temperature rising rate is 2-5 ℃/min before the primary sintering. Preferably, after primary sintering, naturally cooling to obtain a green body.
Preferably, in step (2), the blasting treatment comprises blasting sand balls onto the surface of the green body. Preferably, the sand spheres are selected from boron carbide, zirconia or alumina. Further, the pressure of the sand blasting is 1-10bar; the working distance of the sand blasting is 10-50mm; the moving speed of the sand blasting is 1-20mm/s.
4. A surface treatment method according to any one of claims 1 to 3, wherein in step (2), the etching treatment comprises: and (3) treating the surface of the blank by adopting etching liquid.
Preferably, the etching solution includes a first acid and hydrofluoric acid. Preferably, the first acid may be selected from at least one, two or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and the like.
5. The surface treatment method according to any one of claims 1 to 4, wherein a volume ratio of the hydrofluoric acid and the first acid in the etching liquid is (2 to 8): (8-2).
Preferably, the etching time is 1min-120min.
Preferably, the temperature of the etching is 30-100 ℃.
Preferably, in step (2), the final sintering includes: sintering temperature is 1450-1530 ℃; the sintering time is 1.5h-2.5h.
Preferably, the cleaning is also performed after the blasting, acid etching or final sintering.
6. A surface topography of an implant, characterized in that the surface topography is produced by the surface treatment method according to any one of claims 1-5.
7. The surface topography of an implant of claim 6, wherein the implant comprises at least the following raw materials:
5 to 5.5 weight percent of yttrium oxide,
The hafnium oxide is not more than 5wt%,
88-95% Of zirconia.
Preferably, the surface of the implant has a roughness Ra of 1-5 μm.
8. An implant whose surface comprises the surface topography of the implant of claim 6 or 7.
9. An implant, the surface of which is prepared by the surface treatment method according to any one of claims 1 to 5.
Preferably, the surface of the implant has a roughness Ra of 1-5 μm.
10. Use of the implant of claim 9 in a medical bioimplant material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410625115.3A CN118580067A (en) | 2024-05-20 | 2024-05-20 | Surface treatment method of zirconium oxide implant and its application |
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| CN202410625115.3A CN118580067A (en) | 2024-05-20 | 2024-05-20 | Surface treatment method of zirconium oxide implant and its application |
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| CN202410625115.3A Pending CN118580067A (en) | 2024-05-20 | 2024-05-20 | Surface treatment method of zirconium oxide implant and its application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN120036965A (en) * | 2025-02-07 | 2025-05-27 | 北京瑞瓷医疗科技有限公司 | Integrated high-strength implant and manufacturing method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008009272A1 (en) * | 2006-07-20 | 2008-01-24 | Dieter Keller | Implant |
| CN101707927A (en) * | 2007-07-06 | 2010-05-12 | 维塔假牙制造厂H·劳特有限责任两合公司 | Ceramic body and preparation method thereof |
| US20150125821A1 (en) * | 2012-06-18 | 2015-05-07 | 3M Innovative Properties Company | Process for producing a zirconia based dental implant |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008009272A1 (en) * | 2006-07-20 | 2008-01-24 | Dieter Keller | Implant |
| CN101707927A (en) * | 2007-07-06 | 2010-05-12 | 维塔假牙制造厂H·劳特有限责任两合公司 | Ceramic body and preparation method thereof |
| US20150125821A1 (en) * | 2012-06-18 | 2015-05-07 | 3M Innovative Properties Company | Process for producing a zirconia based dental implant |
Non-Patent Citations (1)
| Title |
|---|
| 丁茜;张磊;孙玉春;谢秋菲;: "不同表面处理方法对CAD/CAM氧化锆种植体表面显微形貌的影响研究", 实用口腔医学杂志, no. 06, 30 November 2016 (2016-11-30) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN120036965A (en) * | 2025-02-07 | 2025-05-27 | 北京瑞瓷医疗科技有限公司 | Integrated high-strength implant and manufacturing method thereof |
| CN120036965B (en) * | 2025-02-07 | 2025-12-05 | 北京瑞瓷医疗科技有限公司 | An integrated high-strength implant and its manufacturing method |
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