CN111803712B - Zirconia ceramic implant with periodic pore structure and preparation method thereof - Google Patents
Zirconia ceramic implant with periodic pore structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a zirconia ceramic implant with a periodic pore structure and a preparation method thereof. The zirconia ceramic implant comprises an upper half part and a lower half part, wherein the raw materials of the upper half part comprise zirconia, alumina, yttrium oxide, silicon dioxide, titanium dioxide, polyethylacryloyl, trimethylolpropane triacrylate, dimethylolpropionic acid and epoxy resin; the raw materials of the lower half part comprise zirconium oxide, aluminum oxide, silicon dioxide, titanium dioxide, hydroxyapatite, sodium silicate, polyethylacryloyl, trimethylolpropane triacrylate, dimethylolpropionic acid and epoxy resin. The preparation method comprises the steps of mixing ceramic matrix powder, premixing an auxiliary agent, preparing an upper half raw material, preparing a lower half raw material, printing a lower half part of the implant, printing an upper half part of the implant and sintering the ceramic implant. The zirconia ceramic implant is solid at the upper half part, hollow at the lower half part and accompanied with a periodic mesh structure, and has high bonding strength with bones, high strength at an occlusion end and high shearing resistance.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to a zirconia ceramic implant with a periodic pore structure and a preparation method thereof.
Background
In recent years, with the widespread use of zirconia materials in the biomedical field, there is a tendency to repair a missing tooth using zirconia as a mesogen. The zirconia belongs to a high molecular biological inert ceramic material, has good biocompatibility, can keep a long-term stable state, and also has clinically acceptable mechanical properties.
The zirconia ceramic implant in the prior art is a single solid body from top to bottom, and in order to ensure the fusion of the implant and bone tissues, the bone tissue fixing implant needs longer time, so that the repair period of the implant is increased, the use amount of the zirconia ceramic material is increased, and the production cost is increased.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects, the invention provides the zirconia ceramic implant with the periodic pore structure and the preparation method thereof, the upper half part of the zirconia ceramic implant is solid, and the lower half part of the zirconia ceramic implant is hollow and is accompanied with the periodic mesh structure, so that the osseointegration can be increased, and the locking strength can be improved; meanwhile, the bite end has high strength and high shearing resistance.
The technical scheme adopted by the invention for solving the technical problems is as follows: the zirconia ceramic implant with the periodic pore structure comprises an upper half part and a lower half part, wherein the upper half part and the lower half part are respectively made of the following raw materials in parts by weight:
the raw materials of the upper half part comprise 100 parts of zirconia, 30-50 parts of alumina, 0.5-5.0 parts of yttrium oxide, 20-50 parts of silicon dioxide, 10-20 parts of titanium dioxide, 0.4-1.2 parts of polyethylacryloyl, 0.5-2.0 parts of trimethylolpropane triacrylate, 2.0-5.0 parts of dimethylolpropionic acid and 80-95 parts of epoxy resin;
the raw materials of the lower half part comprise 100 parts of zirconia, 30-50 parts of alumina, 10-30 parts of silicon dioxide, 5-10 parts of titanium dioxide, 5-10 parts of hydroxyapatite, 0.5-3.0 parts of sodium silicate, 0.4-1.2 parts of polyethylacryloyl, 0.5-2.0 parts of trimethylolpropane triacrylate, 2.0-5.0 parts of dimethylolpropionic acid and 60-80 parts of epoxy resin.
According to the zirconia ceramic implant with the periodic pore structure, zirconia and alumina are adopted as ceramic matrix materials in the ceramic main body, and the ceramic main body has a good synergistic effect with other additives in a proper proportion, so that the ceramic implant has good strength and mechanical properties and good service performance; specifically, the upper half part of the ceramic implant adopts a solid structure and the lower half part of the ceramic implant is hollow and is accompanied with a periodic mesh structure, wherein the upper half part adopts silicon dioxide and titanium dioxide as one of solid phase fillers, the silicon dioxide and the titanium dioxide can permeate into the internal gaps of the zirconia ceramic, the structure density is high, and the compressive strength of the ceramic is effectively improved; the lower half part adopts silicon dioxide, titanium dioxide, hydroxyapatite and sodium silicate as solid-phase fillers, so that the sintered ceramic has holes, the auxiliary agents are uniformly distributed on the surfaces of zirconia and alumina, the sintered zirconia ceramic implant is of a closed porous structure and meets the porosity required by the ceramic implant, the hydroxyapatite is used as a supporting material, and the holes formed after the ceramic slurry which is uniformly mixed is sintered are periodically changed; the lower half part of the ceramic implant is provided with the pore canal, so that the bone tissue can grow inwards to form bone-implant interactive mechanical locking, the bone combination can be increased, and the locking strength can be improved; in addition, the hydroxyapatite is a molding raw material which accords with bone growth factors, can reduce the time required by fixing the ceramic implant by bone tissues, and shortens the repair cycle of the implanted tooth.
Further, the particle size of the silicon dioxide in the upper half part and the lower half part is 100nm-200 nm. The silicon dioxide with the particle size can effectively avoid the agglomeration of silicon dioxide powder in slurry, has excellent surface area, and can be distributed and covered on the surface of a pore channel formed after the sintering of zirconia and alumina, so that the interior of the ceramic implant is of a closed porous structure, and the mechanical property of the ceramic implant is improved.
The preparation method of the zirconia ceramic implant with the periodic pore canal structure comprises the following operation steps,
s1, mixing of ceramic matrix powder: respectively loading alumina and zirconia into a ball mill to obtain zirconia/alumina mixed powder;
s2, premixing auxiliaries: adding polyethylacryloyl, trimethylolpropane triacrylate and dimethylolpropionic acid into a premixer to obtain an auxiliary agent premix, and uniformly mixing for later use;
s3, preparing the upper half raw material: sequentially adding yttrium oxide, silicon dioxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 5-10 minutes to obtain a mixed solution A; taking a half of the auxiliary agent premix obtained in the operation of S2, dropwise adding the half of the auxiliary agent premix into the mixed solution A, and stirring for 10-20 minutes to obtain a mixed solution B; adding half of the mass of the zirconia/alumina mixed powder obtained in the step S1 into the mixed solution B step by step for multiple times, and stirring and mixing for 15-45 minutes to obtain the upper half raw material of the ceramic implant;
s4, preparing the raw materials of the lower half part: sequentially adding silicon oxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 5-10 minutes to obtain a mixed solution C; dropwise adding the residual premixed solution of the auxiliary agent obtained in the step S2 into the mixed solution C, and stirring for 10-20 minutes to obtain a mixed solution D; adding the residual zirconium oxide/aluminum oxide mixed powder obtained in the operation of S1 into the mixed solution D step by step for multiple times, stirring for 5-10 minutes, continuing to add the hydroxyapatite and the sodium silicate into the mixed solution, and stirring and mixing for 15-45 minutes to obtain a lower half part raw material of the ceramic implant;
s5, printing the lower half of the implant: pouring the raw material of the lower half part of the ceramic implant prepared in the step S4 into a first material groove of a 3D printer, and printing to obtain the lower half part of the ceramic implant;
s6, printing the upper half part of the implant: pouring the upper half raw material of the ceramic implant prepared in the step S3 into a second trough of a 3D printer, and continuously printing the upper half part of the ceramic implant layer by layer on the lower half part of the ceramic implant printed in the step S5 to obtain a complete zirconia ceramic blank;
s7, sintering the ceramic implant: and sintering the zirconia ceramic blank obtained in the step S6 to obtain the zirconia ceramic implant.
According to the preparation method of the ceramic implant, the mixing and feeding sequence among different raw materials is limited, so that the characteristics of low viscosity and high solid content of the upper half raw material and the lower half raw material of the mixed implant are ensured, and the precision and the density of the prepared ceramic implant are improved; the printing process is smooth and the operation is simple.
Further, the stirring speed of the ball mill is 200-300 rpm, and the stirring speed of the stirring kettle is 1000-3000 rpm. The proper stirring speed of the ball mill and the stirring kettle is controlled, the dispersion uniformity in the preparation process of the ceramic slurry is ensured, the microstructure of the printed ceramic implant is uniform, the pore channels in the ceramic implant are ensured to be periodically changed, and the quality of the implant is high.
Further, in the S5 lower half-part implant printing operation and the S6 upper half-part implant printing operation, the scraper speed of the 3D printer is 600-1500 step/S; ultraviolet radiation is adopted for curing, and the wavelength of the ultraviolet light is 350-380 nm. The scraper speed of the printer is controlled, so that the slurry cannot be sputtered in the printing process to influence the smoothness inside the printer, the thickness is uniform, and the production rate is ensured; when the successive layer was printed, realize the successive layer and dry, the internal humidity of ceramic planting body of avoiding printing out is uneven, and inside collapses when avoiding follow-up sintering, influences the sintering quality.
Furthermore, the sintering of the S7 ceramic implant adopts microwave vacuum sintering, the sintering temperature is 1430-1500 ℃, the sintering time is 0.5-2h, and the sintering vacuum degree in a microwave sintering furnace is 0.2-200 Pa. The microwave sintering is adopted, so that the method has the advantages of high heating speed, capability of inhibiting the growth of a grain structure, high compactness of the zirconia ceramic implant, difficult cracking, high strength of an occlusion end and high shearing resistance.
The invention has the beneficial effects that:
1. according to the zirconia ceramic implant with the periodic pore structure, zirconia and alumina are adopted as ceramic matrix materials in the ceramic main body, and the ceramic main body has a good synergistic effect with other additives in a proper proportion, so that the ceramic implant has good strength and mechanical properties and good service performance; specifically, the upper half part of the ceramic implant adopts a solid structure and the lower half part of the ceramic implant is hollow and is accompanied with a periodic mesh structure, wherein the upper half part adopts silicon dioxide and titanium dioxide as one of solid phase fillers, the silicon dioxide and the titanium dioxide can permeate into the internal gaps of the zirconia ceramic, the structure density is high, and the compressive strength of the ceramic is effectively improved; the lower half part adopts silicon dioxide, titanium dioxide, hydroxyapatite and sodium silicate as solid-phase fillers, so that the sintered ceramic has holes, the auxiliary agents are uniformly distributed on the surfaces of zirconia and alumina, the sintered zirconia ceramic implant is of a closed porous structure and meets the porosity required by the ceramic implant, the hydroxyapatite is used as a supporting material, and the holes formed after the ceramic slurry which is uniformly mixed is sintered are periodically changed; the lower half part of the ceramic implant is provided with the pore canal, so that the bone tissue can grow inwards to form bone-implant interactive mechanical locking, the bone combination can be increased, and the locking strength can be improved; in addition, the hydroxyapatite is a molding raw material which accords with bone growth factors, so that the time required by fixing the ceramic implant by bone tissues can be reduced, and the repair cycle of the implanted tooth is shortened; the silicon dioxide with the particle size can effectively avoid the agglomeration of silicon dioxide powder in slurry, has excellent surface area, and can be distributed and covered on the surface of a pore channel formed after the sintering of zirconia and alumina, so that the interior of the ceramic implant is of a closed porous structure, and the mechanical property of the ceramic implant is improved.
2. According to the preparation method of the ceramic implant, the mixing and feeding sequence among different raw materials is limited, so that the characteristics of low viscosity and high solid content of the upper half raw material and the lower half raw material of the mixed implant are ensured, and the precision and the density of the prepared ceramic implant are improved; the printing process is smooth, and the operation is simple; the proper stirring speed of the ball mill and the stirring kettle is controlled to ensure the dispersion uniformity in the preparation process of the ceramic slurry, the microstructure of the printed ceramic implant is uniform, the pore channels in the ceramic implant are ensured to be periodically changed, and the implant has high quality; the scraper speed of the printer is controlled, so that the slurry cannot be sputtered in the printing process to influence the smoothness inside the printer, the thickness is uniform, and the production rate is ensured; during layer-by-layer printing, drying layer-by-layer is realized, uneven humidity in the printed ceramic implant is avoided, and internal collapse during subsequent sintering is avoided to influence sintering quality; the microwave sintering is adopted, so that the method has the advantages of high heating speed, capability of inhibiting the growth of a grain structure, high compactness of the zirconia ceramic implant, difficult cracking, high strength of an occlusion end and high shearing resistance.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The zirconia ceramic implant with the periodic pore structure comprises an upper half part and a lower half part, wherein the upper half part and the lower half part are respectively made of the following raw materials in parts by weight:
the raw materials of the upper half part comprise 100 parts of zirconia, 30 parts of alumina, 0.8 part of yttrium oxide, 25 parts of silicon dioxide, 20 parts of titanium dioxide, 0.5 part of polyethylacryloyl, 2.0 parts of trimethylolpropane triacrylate, 4.5 parts of dimethylolpropionic acid and 82 parts of epoxy resin;
the raw materials of the lower half part comprise 100 parts of zirconia, 30 parts of alumina, 12 parts of silicon dioxide, 10 parts of titanium dioxide, 6 parts of hydroxyapatite, 0.5 part of sodium silicate, 0.5 part of polyethylacryloyl, 2.0 parts of trimethylolpropane triacrylate, 4.5 parts of dimethylolpropionic acid and 78 parts of epoxy resin.
The particle sizes of the silicon dioxide in the upper half part and the lower half part are both 100nm-200 nm.
The preparation method of the zirconia ceramic implant with the periodic pore canal structure comprises the following operation steps,
s1, mixing of ceramic matrix powder: respectively loading alumina and zirconia into a ball mill, wherein the stirring speed of the ball mill is 220rpm, so as to obtain zirconia/alumina mixed powder;
s2, premixing auxiliaries: adding polyethylacryloyl, trimethylolpropane triacrylate and dimethylolpropionic acid into a premixer to obtain an auxiliary agent premix, and uniformly mixing for later use;
s3, preparing the upper half raw material: sequentially adding yttrium oxide, silicon dioxide and titanium dioxide into a stirring kettle filled with epoxy resin in parts by weight, wherein the stirring speed of the stirring kettle is 3000rpm, and mixing and stirring for 5 minutes to obtain a mixed solution A; taking a half of the auxiliary agent premix obtained in the operation of S2, dropwise adding the half of the auxiliary agent premix into the mixed solution A, and stirring for 15 minutes to obtain a mixed solution B; adding half of the mass of the zirconia/alumina mixed powder obtained in the step S1 into the mixed solution B step by step for multiple times, and stirring and mixing for 20 minutes to obtain the upper half raw material of the ceramic implant;
s4, preparing the raw materials of the lower half part: sequentially adding silicon oxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 5 minutes to obtain a mixed solution C; dropwise adding the rest premixed solution of the auxiliary agent obtained in the step S2 into the mixed solution C, and stirring for 15 minutes to obtain a mixed solution D; adding the residual zirconium oxide/aluminum oxide mixed powder obtained in the operation of S1 into the mixed solution D step by step for multiple times, stirring for 5 minutes, continuing to add the hydroxyapatite and the sodium silicate into the mixed solution, and stirring and mixing for 20 minutes to obtain a lower half part raw material of the ceramic implant;
s5, printing the lower half of the implant: pouring the raw material of the lower half part of the ceramic implant prepared in the step S4 into a first material groove of a 3D printer, and printing to obtain the lower half part of the ceramic implant; the scraper speed of the 3D printer is 800 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 355 nm;
s6, printing the upper half part of the implant: pouring the upper half raw material of the ceramic implant prepared in the step S3 into a second trough of a 3D printer, and continuously printing the upper half part of the ceramic implant layer by layer on the lower half part of the ceramic implant printed in the step S5 to obtain a complete zirconia ceramic blank; the scraper speed of the 3D printer is 800 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 355 nm;
s7, sintering the ceramic implant: sintering the zirconia ceramic blank obtained in the operation of S6, wherein the sintering adopts microwave vacuum sintering, the sintering temperature is 1430-1500 ℃, the sintering time is 1.0h, and the sintering vacuum degree in a microwave sintering furnace is 100Pa, so as to obtain the zirconia ceramic implant.
Example 2
The zirconia ceramic implant with the periodic pore structure comprises an upper half part and a lower half part, wherein the upper half part and the lower half part are respectively made of the following raw materials in parts by weight:
the raw materials of the upper half part comprise 100 parts of zirconia, 36 parts of alumina, 2.0 parts of yttrium oxide, 30 parts of silicon dioxide, 15 parts of titanium dioxide, 1.2 parts of polyethylacryloyl, 1.0 part of trimethylolpropane triacrylate, 3.6 parts of dimethylolpropionic acid and 92 parts of epoxy resin;
the raw materials of the lower half part comprise 100 parts of zirconium oxide, 36 parts of aluminum oxide, 18 parts of silicon dioxide, 6 parts of titanium dioxide, 8 parts of hydroxyapatite, 1.5 parts of sodium silicate, 1.2 parts of polyethylacryloyl, 1.0 part of trimethylolpropane triacrylate, 3.6 parts of dimethylolpropionic acid and 80 parts of epoxy resin.
The particle sizes of the silicon dioxide in the upper half part and the lower half part are both 100nm-200 nm.
The preparation method of the zirconia ceramic implant with the periodic pore canal structure comprises the following operation steps,
s1, mixing of ceramic matrix powder: respectively loading alumina and zirconia into a ball mill, wherein the stirring speed of the ball mill is 300rpm, so as to obtain zirconia/alumina mixed powder;
s2, premixing auxiliaries: adding polyethylacryloyl, trimethylolpropane triacrylate and dimethylolpropionic acid into a premixer to obtain an auxiliary agent premix, and uniformly mixing for later use;
s3, preparing the upper half raw material: sequentially adding yttrium oxide, silicon dioxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, wherein the stirring speed of the stirring kettle is 2500rpm, and mixing and stirring for 6 minutes to obtain a mixed solution A; taking a half of the auxiliary agent premix obtained in the operation of S2, dropwise adding the half of the auxiliary agent premix into the mixed solution A, and stirring for 12 minutes to obtain a mixed solution B; adding half of the mass of the zirconia/alumina mixed powder obtained in the step S1 into the mixed solution B step by step for multiple times, and stirring and mixing for 20 minutes to obtain the upper half raw material of the ceramic implant;
s4, preparing the raw materials of the lower half part: sequentially adding silicon oxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 6 minutes to obtain a mixed solution C; dropwise adding the rest premixed solution of the auxiliary agent obtained in the step S2 into the mixed solution C, and stirring for 12 minutes to obtain a mixed solution D; adding the residual zirconium oxide/aluminum oxide mixed powder obtained in the operation of S1 into the mixed solution D step by step for multiple times, stirring for 6 minutes, continuing to add the hydroxyapatite and the sodium silicate into the mixed solution, and stirring and mixing for 20 minutes to obtain a lower half part raw material of the ceramic implant;
s5, printing the lower half of the implant: pouring the raw material of the lower half part of the ceramic implant prepared in the step S4 into a first material groove of a 3D printer, and printing to obtain the lower half part of the ceramic implant; the scraper speed of the 3D printer is 1000 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 355 nm;
s6, printing the upper half part of the implant: pouring the upper half raw material of the ceramic implant prepared in the step S3 into a second trough of a 3D printer, and continuously printing the upper half part of the ceramic implant layer by layer on the lower half part of the ceramic implant printed in the step S5 to obtain a complete zirconia ceramic blank; the scraper speed of the 3D printer is 1000 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 355 nm;
s7, sintering the ceramic implant: sintering the zirconia ceramic blank obtained in the operation of S6, wherein the sintering adopts microwave vacuum sintering, the sintering temperature is 1430-1500 ℃, the sintering time is 1.2h, and the sintering vacuum degree in a microwave sintering furnace is 50Pa, so as to obtain the zirconia ceramic implant.
Example 3
The zirconia ceramic implant with the periodic pore structure comprises an upper half part and a lower half part, wherein the upper half part and the lower half part are respectively made of the following raw materials in parts by weight:
the raw materials of the upper half part comprise 100 parts of zirconia, 41 parts of alumina, 3.6 parts of yttrium oxide, 46 parts of silicon dioxide, 10 parts of titanium dioxide, 1.0 part of polyethylacryloyl, 0.8 part of trimethylolpropane triacrylate, 4.0 parts of dimethylolpropionic acid and 92 parts of epoxy resin;
the raw materials of the lower half part comprise 100 parts of zirconium oxide, 41 parts of aluminum oxide, 25 parts of silicon dioxide, 8 parts of titanium dioxide, 6 parts of hydroxyapatite, 2.4 parts of sodium silicate, 1.0 part of polyethylacryloyl, 0.8 part of trimethylolpropane triacrylate, 4.0 parts of dimethylolpropionic acid and 66 parts of epoxy resin.
The particle sizes of the silicon dioxide in the upper half part and the lower half part are both 100nm-200 nm.
The preparation method of the zirconia ceramic implant with the periodic pore canal structure comprises the following operation steps,
s1, mixing of ceramic matrix powder: respectively loading alumina and zirconia into a ball mill, wherein the stirring speed of the ball mill is 200rpm, so as to obtain zirconia/alumina mixed powder;
s2, premixing auxiliaries: adding polyethylacryloyl, trimethylolpropane triacrylate and dimethylolpropionic acid into a premixer to obtain an auxiliary agent premix, and uniformly mixing for later use;
s3, preparing the upper half raw material: sequentially adding yttrium oxide, silicon dioxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, wherein the stirring speed of the stirring kettle is 1500rpm, and mixing and stirring for 8 minutes to obtain a mixed solution A; taking a half of the auxiliary agent premix obtained in the operation of S2, dropwise adding the half of the auxiliary agent premix into the mixed solution A, and stirring for 15 minutes to obtain a mixed solution B; adding half of the mass of the zirconia/alumina mixed powder obtained in the step S1 into the mixed solution B step by step for multiple times, and stirring and mixing for 40 minutes to obtain the upper half raw material of the ceramic implant;
s4, preparing the raw materials of the lower half part: sequentially adding silicon oxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 8 minutes to obtain a mixed solution C; dropwise adding the rest premixed solution of the auxiliary agent obtained in the step S2 into the mixed solution C, and stirring for 15 minutes to obtain a mixed solution D; adding the residual zirconium oxide/aluminum oxide mixed powder obtained in the operation of S1 into the mixed solution D step by step for multiple times, stirring for 8 minutes, continuing to add the hydroxyapatite and the sodium silicate into the mixed solution, and stirring and mixing for 45 minutes to obtain a lower half part raw material of the ceramic implant;
s5, printing the lower half of the implant: pouring the raw material of the lower half part of the ceramic implant prepared in the step S4 into a first material groove of a 3D printer, and printing to obtain the lower half part of the ceramic implant; the scraper speed of the 3D printer is 600 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 365 nm;
s6, printing the upper half part of the implant: pouring the upper half raw material of the ceramic implant prepared in the step S3 into a second trough of a 3D printer, and continuously printing the upper half part of the ceramic implant layer by layer on the lower half part of the ceramic implant printed in the step S5 to obtain a complete zirconia ceramic blank; the scraper speed of the 3D printer is 600 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 365 nm;
s7, sintering the ceramic implant: sintering the zirconia ceramic blank obtained in the operation of S6, wherein the sintering adopts microwave vacuum sintering, the sintering temperature is 1430-1500 ℃, the sintering time is 2h, and the sintering vacuum degree in a microwave sintering furnace is 200Pa, so as to obtain the zirconia ceramic implant.
Example 4
The zirconia ceramic implant with the periodic pore structure comprises an upper half part and a lower half part, wherein the upper half part and the lower half part are respectively made of the following raw materials in parts by weight:
the raw materials of the upper half part comprise 100 parts of zirconia, 50 parts of alumina, 4.5 parts of yttrium oxide, 20 parts of silicon dioxide, 20 parts of titanium dioxide, 1.2 parts of polyethylacryloyl, 0.5 part of trimethylolpropane triacrylate, 5.0 parts of dimethylolpropionic acid and 80 parts of epoxy resin;
the raw materials of the lower half part comprise 100 parts of zirconium oxide, 50 parts of aluminum oxide, 30 parts of silicon dioxide, 5 parts of titanium dioxide, 10 parts of hydroxyapatite, 2.8 parts of sodium silicate, 1.2 parts of polyethylacryloyl, 0.5 part of trimethylolpropane triacrylate, 5.0 parts of dimethylolpropionic acid and 60 parts of epoxy resin.
The particle sizes of the silicon dioxide in the upper half part and the lower half part are both 100nm-200 nm.
The preparation method of the zirconia ceramic implant with the periodic pore canal structure comprises the following operation steps,
s1, mixing of ceramic matrix powder: respectively loading alumina and zirconia into a ball mill, wherein the stirring speed of the ball mill is 250rpm, so as to obtain zirconia/alumina mixed powder;
s2, premixing auxiliaries: adding polyethylacryloyl, trimethylolpropane triacrylate and dimethylolpropionic acid into a premixer to obtain an auxiliary agent premix, and uniformly mixing for later use;
s3, preparing the upper half raw material: sequentially adding yttrium oxide, silicon dioxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, wherein the stirring speed of the stirring kettle is 1600rpm, and mixing and stirring for 8 minutes to obtain a mixed solution A; taking a half of the auxiliary agent premix obtained in the operation of S2, dropwise adding the half of the auxiliary agent premix into the mixed solution A, and stirring for 15 minutes to obtain a mixed solution B; adding half of the mass of the zirconia/alumina mixed powder obtained in the step S1 into the mixed solution B step by step for multiple times, and stirring and mixing for 30 minutes to obtain the upper half raw material of the ceramic implant;
s4, preparing the raw materials of the lower half part: sequentially adding silicon oxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 8 minutes to obtain a mixed solution C; dropwise adding the rest premixed solution of the auxiliary agent obtained in the step S2 into the mixed solution C, and stirring for 15 minutes to obtain a mixed solution D; adding the residual zirconium oxide/aluminum oxide mixed powder obtained in the operation of S1 into the mixed solution D step by step for multiple times, stirring for 6 minutes, continuing to add the hydroxyapatite and the sodium silicate into the mixed solution, and stirring and mixing for 30 minutes to obtain a lower half part raw material of the ceramic implant;
s5, printing the lower half of the implant: pouring the raw material of the lower half part of the ceramic implant prepared in the step S4 into a first material groove of a 3D printer, and printing to obtain the lower half part of the ceramic implant; the scraper speed of the 3D printer is 800 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 355 nm;
s6, printing the upper half part of the implant: pouring the upper half raw material of the ceramic implant prepared in the step S3 into a second trough of a 3D printer, and continuously printing the upper half part of the ceramic implant layer by layer on the lower half part of the ceramic implant printed in the step S5 to obtain a complete zirconia ceramic blank; the scraper speed of the 3D printer is 800 step/s; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 355 nm;
s7, sintering the ceramic implant: sintering the zirconia ceramic blank obtained in the operation of S6, wherein the sintering adopts microwave vacuum sintering, the sintering temperature is 1430-1500 ℃, the sintering time is 1h, and the sintering vacuum degree in a microwave sintering furnace is 100Pa, so as to obtain the zirconia ceramic implant.
In the examples 1-4, the pore channels of the zirconia ceramic implant are periodically changed through electron microscope observation, and the performance test is carried out on the zirconia ceramic implant, so that the yield strength of the examples 1-4 is greater than 580MPa, the elongation is 14.2%, the mechanical property is good, and the service life is long.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (3)
1. The preparation method of the zirconia ceramic implant with the periodic pore structure is characterized in that the ceramic implant comprises an upper half part and a lower half part, wherein the upper half part and the lower half part are respectively prepared from the following raw materials in parts by weight:
the raw materials of the upper half part comprise 100 parts of zirconia, 30-50 parts of alumina, 0.5-5.0 parts of yttrium oxide, 20-50 parts of silicon dioxide, 10-20 parts of titanium dioxide, 0.4-1.2 parts of polyethylacryloyl, 0.5-2.0 parts of trimethylolpropane triacrylate, 2.0-5.0 parts of dimethylolpropionic acid and 80-95 parts of epoxy resin;
the raw materials of the lower half part comprise 100 parts of zirconia, 30-50 parts of alumina, 10-30 parts of silicon dioxide, 5-10 parts of titanium dioxide, 5-10 parts of hydroxyapatite, 0.5-3.0 parts of sodium silicate, 0.4-1.2 parts of polyethylacryloyl, 0.5-2.0 parts of trimethylolpropane triacrylate, 2.0-5.0 parts of dimethylolpropionic acid and 60-80 parts of epoxy resin;
the preparation method comprises the following operation steps of,
s1, mixing of ceramic matrix powder: respectively loading alumina and zirconia into a ball mill to obtain zirconia/alumina mixed powder;
s2, premixing auxiliaries: adding polyethylacryloyl, trimethylolpropane triacrylate and dimethylolpropionic acid into a premixer to obtain an auxiliary agent premix, and uniformly mixing for later use;
s3, preparing the upper half raw material: sequentially adding yttrium oxide, silicon dioxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 5-10 minutes to obtain a mixed solution A; taking a half of the auxiliary agent premix obtained in the operation of S2, dropwise adding the half of the auxiliary agent premix into the mixed solution A, and stirring for 10-20 minutes to obtain a mixed solution B; adding half of the mass of the zirconia/alumina mixed powder obtained in the step S1 into the mixed solution B step by step for multiple times, and stirring and mixing for 15-45 minutes to obtain the upper half raw material of the ceramic implant;
s4, preparing the raw materials of the lower half part: sequentially adding silicon dioxide and titanium dioxide into a stirring kettle filled with the calculated parts of epoxy resin, and mixing and stirring for 5-10 minutes to obtain a mixed solution C; dropwise adding the residual premixed solution of the auxiliary agent obtained in the step S2 into the mixed solution C, and stirring for 10-20 minutes to obtain a mixed solution D; adding the residual zirconium oxide/aluminum oxide mixed powder obtained in the operation of S1 into the mixed solution D step by step for multiple times, stirring for 5-10 minutes, continuing to add hydroxyapatite and sodium silicate into the mixed solution, stirring and mixing for 15-45 minutes, and obtaining the lower half part raw material of the ceramic implant;
s5, printing the lower half of the implant: pouring the raw material of the lower half part of the ceramic implant prepared in the step S4 into a first material groove of a 3D printer, and printing to obtain the lower half part of the ceramic implant;
s6, printing the upper half part of the implant: pouring the upper half raw material of the ceramic implant prepared in the step S3 into a second trough of a 3D printer, and continuously printing the upper half part of the ceramic implant layer by layer on the lower half part of the ceramic implant printed in the step S5 to obtain a complete zirconia ceramic blank;
s7, sintering the ceramic implant: sintering the zirconia ceramic blank obtained in the operation of S6 to obtain a zirconia ceramic implant;
in the S5 lower half part printing operation and the S6 upper half part printing operation of the implant, the scraper speed of the 3D printer is 600-1500 steps/S; curing by adopting ultraviolet irradiation, wherein the wavelength of the ultraviolet light is 350-380 nm;
the sintering of the S7 ceramic implant adopts microwave vacuum sintering, the sintering temperature is 1430-1500 ℃, the sintering time is 0.5-2h, and the sintering vacuum degree in a microwave sintering furnace is 0.2-200 Pa.
2. The method for preparing a zirconia ceramic implant with a periodic pore structure according to claim 1, wherein: the particle sizes of the silicon dioxide in the upper half part and the lower half part are both 100nm-200 nm.
3. The method for preparing a zirconia ceramic implant with a periodic pore structure according to claim 1, wherein: the stirring speed of the ball mill is 200-300 rpm, and the stirring speed of the stirring kettle is 1000-3000 rpm.
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Denomination of invention: Zirconia ceramic implant with periodic pore structure and its preparation method Effective date of registration: 20221026 Granted publication date: 20220422 Pledgee: Zhejiang Jiashan rural commercial bank Limited by Share Ltd. science and technology sub branch Pledgor: Jiaxing raoji Technology Co.,Ltd. Registration number: Y2022450000185 |