Patent ID: 12195835

DETAILED DESCRIPTION

For clearer technical methods, advantages and objects of the present application, the technical solutions of the present application will be described in detail below. However, the described content is only preferred embodiments of the present application. Without departing from the spirit and concept of the present application, any modification or replacement of the steps or conditions of the present application shall fall within the protection scope of the present application.

Comparative Examples 1 and 2

Comparative Example 1 provides a magnesium-zinc-manganese alloy bar formed by hot extrusion, and only under the action of single alternating magnetic field, the magnesium-zinc-manganese alloy bar has a tensile mechanical property as shown by curve 3 inFIG.1. Comparative Example 2 provides a magnesium-zinc-manganese alloy bar formed by hot extrusion, and after room-temperature rotary forging in conjunction with cryogenic processing, the magnesium-zinc-manganese alloy bar has a tensile mechanical property as shown by curve 2 inFIG.1. The magnesium alloy bar obtained in Comparative Example 1 was mechanically processed into a bone screw product, and the bone screw product was degraded in simulated body fluid for 15 days, the corrosion degree of which is shown inFIG.9(1)(2).

Example 1

A method for preparing a magnesium alloy bone screw bar via room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing includes the following steps:S1: preparing an ingot: magnesium-zinc-manganese alloy was cast into an ingot, wherein the ingot had a composition satisfying that: 1.5% of Zn, 1.2% of Mn, Si≤0.01, Al≤0.01, Fe≤0.01, Cu≤0.002, Ni≤0.001, and a remainder of Mg; a grain size was controlled at less than or equal to 100 μm;S2: preparing a magnesium-zinc-manganese alloy bar: the ingot was held at 420° C. for 24 h, and then extruded with an extrusion ratio controlled at 40 to obtain a magnesium-zinc-manganese alloy bar with a grain size of 20-30 μm;S3: performing cryogenic processing: the magnesium-zinc-manganese alloy bar was subjected to cryogenic processing for 12 h at a liquid nitrogen temperature controlled at −215° C., and returned to room temperature after the cryogenic processing to obtain a cryogenic processing magnesium-zinc-manganese alloy bar;S4: performing room-temperature rotary forging under alternating magnetic field: the cryogenic processing magnesium-zinc-manganese alloy bar was applied with alternating magnetic field of 10000 Hz by an alternating magnetic field generator of Bamac Electric, and simultaneously subjected to room-temperature rotary forging in a rotary forging machine with a deformation controlled at 50%; the force of rotary forging was applied along with the action of alternating magnetic field to obtain a room-temperature rotary forging magnesium-zinc-manganese alloy bar;S5: steps S3-S4 were repeated until the magnesium-zinc-manganese alloy bar was rotary-forged to a required diameter; andS6: performing subsequent heat processing: the magnesium-zinc-manganese alloy bar obtained in step S5 was placed in an electric furnace at 375° C. and held for 2 h, and then cooled to room temperature to obtain the magnesium alloy bone screw bar.

In the method, the last room-temperature rotary forging had a deformation of 26.5%, guaranteeing sufficient room-temperature deformation to achieve work hardening effect; the microstructure is shown inFIG.3-FIG.7.FIG.2shows the microstructure of magnesium alloy under the action of single alternating magnetic field, and it can be observed that the magnesium alloy has an equiaxial recrystallization structure and the grain size is not uniform; the single alternating magnetic field can be beneficial to the plastic deformation of magnesium alloy, but have limited effect to improve its strength. After room-temperature rotary forging under alternating magnetic field, the grains are obviously broken, the grains are further refined, and especially the subgrains are refined, thus obtaining the effect that the strength is improved by grain refinement (FIG.3); then after cryogenic processing, the morphology of such fine grains can be effectively guaranteed (FIG.4), which thus facilitates the subsequent plastic deformation and strength improvement. After room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing, the dislocations of magnesium alloy generated by plastic deformation can interact with grain boundaries, other dislocations, and second phases (FIG.5-FIG.7), improving the strengthening effect on the magnesium alloy, and under the cryogenic action, such strengthening effect can be further maintained stably, and such strengthening effect can be manifested as improving the wear resistance and bite force of the magnesium alloy bone screw product when rotating in the animal bone.

A tensile curve of the magnesium alloy bone screw bar obtained in this example is shown by curve 1 inFIG.1. From the comparison of curve 1, curve 2 and curve 3 inFIG.1, it can be seen that the plastic deformation capacity of magnesium alloy is greatly improved by the method of room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing. As shown by curve 3, the plastic elongation of magnesium alloy reaches 22% under the action of single alternating magnetic field; with respect to curve 2, after room-temperature rotary forging in conjunction with cryogenic processing, the elongation of magnesium alloy is about 14%, but the strength is increased to 208.4 MPa from 171.2 MPa; with respect to curve 1, via performing room-temperature rotary forging along with alternating magnetic field and combining with cryogenic processing, the elongation of magnesium alloy can reach nearly 60%, thus achieving large plastic deformation, and meanwhile, the strength can reach 268.7 MPa. Therefore, the performance shown by curve 1, whether strength or plasticity, is not a simple superposition of the strength or plasticity of curve 2 and curve 3, but a qualitative leap, that is, a synergistic effect. Specifically, the strength can be improved by 57% and 29% via the method of room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing (curve 1) compared with the single alternating magnetic field (curve 3) and the room-temperature rotary forging in conjunction with cryogenic processing (curve 2), respectively; the elongation is increased by 2.7 times and 4.2 times respectively. In general, the strength and plasticity of the material are significantly improved simultaneously by the room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing, and the synergistic effect is remarkable.

The magnesium alloy bone screw bar obtained from the above preparation method was mechanically processed into a magnesium alloy bone screw product, which had a screw shape with thread, and a length of 20 mm and a diameter of 4 mm, as shown inFIG.8(1).

As shown inFIG.9,FIG.9(1)(2) show the corrosion situation of the bone screw products after soaked in simulated body fluid for 15 days, which are obtained from the magnesium alloy bar after alternating magnetic field in Comparative Example 1;FIG.9(3)(4) show the corrosion situation of the bone screw products after soaked in simulated body fluid for 15 days, which are obtained from the magnesium alloy bar after room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing in this example; the bone screw products shown inFIG.9(1) andFIG.9(3) both have a diameter of 1 mm and a length of 14 mm, and the bone screw products shown inFIG.9(2) andFIG.9(4) both have a diameter of 4 mm and a length of 20 mm. It can be seen from the comparison that after soaked in simulated body fluid for 15 days, the magnesium alloy bone screw products obtained only via alternating magnetic field are obviously corroded, while the magnesium alloy bone screw products obtained via room-temperature rotary forging under alternating magnetic field in conjunction with the cryogenic processing are not corroded.

Example 2

A method for preparing a magnesium alloy bone screw bar via room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing includes the following steps:S1: preparing an ingot: magnesium-zinc-manganese alloy was cast into an ingot, wherein the ingot had a composition satisfying that: 0.5% of Zn, 0.2% of Mn, Si≤0.01, Al≤0.01, Fe≤0.01, Cu≤0.002, Ni≤0.001, and a remainder of Mg; a grain size was controlled at less than or equal to 200 μm;S2: preparing a magnesium-zinc-manganese alloy bar: the ingot was held at 380° C. for 3 h, and then extruded with an extrusion ratio controlled at 16 to obtain a magnesium-zinc-manganese alloy bar with a grain size of less than or equal to 50 μm;S3: performing cryogenic processing: the magnesium-zinc-manganese alloy bar was subjected to cryogenic processing for 1 h at a liquid nitrogen temperature controlled at −195° C., and returned to room temperature after the cryogenic processing to obtain a cryogenic processing magnesium-zinc-manganese alloy bar;S4: performing room-temperature rotary forging under alternating magnetic field: the cryogenic processing magnesium-zinc-manganese alloy bar was applied with alternating magnetic field of 1000 Hz by an alternating magnetic field generator of Bamac Electric, and simultaneously subjected to room-temperature rotary forging in a rotary forging machine with a deformation controlled at 5%; the force of rotary forging was applied along with the action of alternating magnetic field to obtain a room-temperature rotary forging magnesium-zinc-manganese alloy bar;S5: steps S3-S4 were repeated until the magnesium-zinc-manganese alloy bar was rotary-forged to a required diameter; andS6: performing subsequent heat processing: the magnesium-zinc-manganese alloy bar obtained in step S5 was placed in an electric furnace at 275° C. and held for 1 h, and then cooled to room temperature to obtain the magnesium alloy bone screw bar.

In the method, the last room-temperature rotary forging had a deformation of 20.6%, guaranteeing sufficient room-temperature deformation to achieve work hardening effect.

The magnesium alloy bone screw bar obtained from the above preparation method was mechanically processed into a magnesium alloy bone screw product, which had a screw shape with thread, and a length of 14 mm and a diameter of 1 mm, as shown inFIG.8(2).

Example 3

A method for preparing a magnesium alloy bone screw bar via room-temperature rotary forging under alternating magnetic field in conjunction with cryogenic processing includes the following steps:S1: preparing an ingot: magnesium-zinc-manganese alloy was cast into an ingot, wherein the ingot had a composition satisfying that: 1.0% of Zn, 0.6% of Mn, Si≤0.01, Al≤0.01, Fe≤0.01, Cu≤0.002, Ni≤0.001, and a remainder of Mg; a grain size was controlled at less than or equal to 100 μm;S2: preparing a magnesium-zinc-manganese alloy bar: the ingot was held at 400° C. for 12 h, and then extruded with an extrusion ratio controlled at 16 to obtain a magnesium-zinc-manganese alloy bar with a grain size of less than or equal to 50 pin;S3: performing cryogenic processing: the magnesium-zinc-manganese alloy bar was subjected to cryogenic processing for 6 h at a liquid nitrogen temperature controlled at −196° C., and returned to room temperature after the cryogenic processing to obtain a cryogenic processing magnesium-zinc-manganese alloy bar;S4: performing room-temperature rotary forging under alternating magnetic field: the cryogenic processing magnesium-zinc-manganese alloy bar was applied with alternating magnetic field of 5000 Hz by an alternating magnetic field generator of Bamac Electric, and simultaneously subjected to room-temperature rotary forging in a rotary forging machine with a deformation controlled at 35%; the force of rotary forging was applied along with the action of alternating magnetic field to obtain a room-temperature rotary forging magnesium-zinc-manganese alloy bar;S5: steps S3-S4 were repeated until the magnesium-zinc-manganese alloy bar was rotary-forged to a required diameter; andS6: performing subsequent heat processing: the magnesium-zinc-manganese alloy bar obtained in step S5 was placed in an electric furnace at 375° C. and held for 12 h, and then cooled to room temperature to obtain the magnesium alloy bone screw bar.

In the method, the last room-temperature rotary forging had a deformation of 50%, guaranteeing sufficient room-temperature deformation to achieve work hardening effect.

The magnesium alloy bone screw bar obtained from the above preparation method was mechanically processed into a magnesium alloy bone screw product, which had a screw shape with thread, and a length of 18 mm and a diameter of 4 mm, as shown inFIG.8(3).

Furthermore, the magnesium alloy bone screw bar was subjected to cryogenic processing again before the mechanical processing, wherein it was cooled to −196° C. and held for 6 h.

The examples of the present application have been described in detail. However, the described content is only preferred examples of the present application, and the protection scope of the present application is not limited thereto. On the basis of the present application, any modification or improvement which is obvious for those skilled in the art shall fall within the protection scope of the present application.