Manufacturing process of biological ceramic material for implant jointTechnical Field
The application relates to the field of biological joint manufacturing, in particular to a manufacturing process of an implanted joint biological ceramic material.
Background
Hydroxyapatite, abbreviated as HAP, is a surface active material, and since the main component of biological hard tissues (teeth, bones) is hydroxyapatite, hydroxyapatite ceramics are also called artificial bones. The advantages are that: the bone-free composite material has the characteristics of good biological activity and biocompatibility, no toxicity, no rejection reaction, no cancerogenesis, degradability, direct combination with bone and the like, is basically consistent with the structure of human bone crystal components, can be used as a filling material of bone defects, can provide a support for the formation of new bones, plays a role of bone conduction, and is an ideal hard tissue substitute material.
However, it also has the following problems: low strength and high brittleness; the limitation of the defects of low flexural strength, poor toughness and mechanical property and the like influences the wide application of the alloy in medical clinic. The zirconia ceramic material has high strength, high toughness and high hardness, and can well make up the defects of the zirconia ceramic material. The application provides a manufacturing process of the biological ceramic material for the implanted joint.
Disclosure of Invention
In order to solve the problems of low strength and high brittleness of the hydroxyapatite, the application provides a manufacturing process of an implanted joint biological ceramic material.
The manufacturing process of the biological ceramic material for the implanted joint provided by the application adopts the following technical scheme:
the manufacturing process of the biological ceramic material for the implanted joint comprises the following steps,
s1, caHPO is carried out4 With CaC03 According to the following steps: 4, mixing the materials in a molar ratio until a mixture of the two materials is obtained;
s2, performing wet ball milling for 24 hours;
s3, pouring the ball-milled slurry into a container, adding distilled water, stirring at the constant temperature of 80-100 ℃, standing for precipitation after the reaction is finished to obtain a white hydroxyapatite precipitate
6CaHPO4 +4CaC03 A Ca10 (PO4 )6(OH)2 +4C02 +2H2 0；
S4, filtering the precipitated hydroxyapatite, and drying the filtered hydroxyapatite;
s5, ball milling is carried out on the dried hydroxyapatite;
s6, sieving to obtain hydroxyapatite powder;
s7, adding zirconium oxychloride and sodium hydroxide into ionic liquid-sodium trifluoromethylsulfonate for reaction, wherein the reaction temperature is 260-300 ℃, the operating pressure is normal pressure, and the reaction time is 4-20 hours;
s8, after the reaction is finished, cleaning and separating a reaction product, and performing high-temperature treatment on the obtained solid to obtain zirconia powder;
s9, ball milling is carried out on the zirconia powder;
s10, sieving the zirconia split after ball milling;
s11, mixing the powder screened in the S6 and the S10 with resin, putting the mixture into a die, and exhausting under negative pressure;
s12, placing the die into a sintering furnace for sintering;
and S13, demolding after sintering, and polishing from large to small in fineness to finish joint manufacturing.
Preferably, in the wet ball milling in the step S2, the ratio of the steel balls to the materials to the water is 4:2:1, and the granularity of the product after ball milling is D50 less than or equal to 3 mu m.
Preferably, in S6 and S10, the particles with the granularity D50 of more than 5 μm are screened out by sieving.
Preferably, in S11, the mass mixing ratio of zirconia, hydroxyapatite and resin is 1:2:0.5.
Preferably, the number of grinding and polishing in S12 is selected as follows: 600. 800, 1200, 1500, 2000, 500, 0.5 μm polishing paste.
In summary, the present application includes at least one of the following beneficial technical effects:
the zirconia powder, the hydroxyapatite and the resin are fused and highly calcined to obtain the mixture with high strength, high hardness, low brittleness and high toughness, and meanwhile, the mixture has good compatibility with human bodies, so that the popularization and application degree of the mixture in biological materials are improved.
Detailed Description
The present application will be described in further detail below.
The embodiment of the application discloses a manufacturing process of an implanted joint biological ceramic material.
The manufacturing process of the biological ceramic material for the implanted joint comprises the following steps,
s1, caHPO is carried out4 With CaC03 According to the following steps: 4, mixing the materials in a molar ratio until a mixture of the two materials is obtained;
s2, performing wet ball milling for 24 hours, wherein in the wet ball milling, the ratio of steel balls to materials to water is 4:2:1, and the granularity of a product after ball milling is D50 less than or equal to 3 mu m;
s3, pouring the ball-milled slurry into a container, adding distilled water, stirring at the constant temperature of 80-100 ℃, standing for precipitation after the reaction is finished to obtain a white hydroxyapatite precipitate
6CaHPO4 +4CaC03 A Ca10 (PO4 )6(OH)2 +4C02 +2H2 0；
S4, filtering the precipitated hydroxyapatite, and drying the filtered hydroxyapatite;
s5, ball milling is carried out on the dried hydroxyapatite;
s6, sieving to obtain hydroxyapatite powder, and sieving to remove particles with the granularity D50 of more than 5 mu m;
s7, adding zirconium oxychloride and sodium hydroxide into ionic liquid-sodium trifluoromethylsulfonate for reaction, wherein the reaction temperature is 260-300 ℃, the operating pressure is normal pressure, and the reaction time is 4-20 hours;
s8, after the reaction is finished, cleaning and separating a reaction product, and performing high-temperature treatment on the obtained solid to obtain zirconia powder;
s9, ball milling is carried out on the zirconia powder;
s10, sieving the ball-milled zirconia in a split mode, and sieving particles with the granularity D50 of more than 5 mu m;
s11, mixing the powder screened in the steps S6 and S10 with resin, putting the mixture into a die, and exhausting under negative pressure, wherein the mass mixing ratio of zirconia, hydroxyapatite and the resin is 1:2:0.5;
s12, placing the die into a sintering furnace for sintering, and selecting the polishing mesh number as follows: 600. 800, 1200, 1500, 2000, 500, 0.5 μm polishing paste;
and S13, demolding after sintering, and polishing from large to small in fineness to finish joint manufacturing.
It should be noted that in this document, terms such as "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the application, the scope of which is defined in the appended claims and their equivalents.