A medical silicon nitride ceramic material and its preparation method

Abstract

This invention discloses a medical silicon nitride ceramic material and its preparation method. The medical silicon nitride ceramic material is prepared from the following raw materials in the following percentages: 80%–88% silicon nitride powder, 6%–10% sintering aid, 1%–2% carbon nanotubes, 2%–3% nano zinc oxide, 1%–2% nano titanium carbide, and 2%–3% nano zirconium oxide. By limiting the amount of each raw material, this invention enables the prepared medical silicon nitride ceramic material to possess excellent mechanical properties. Specifically, the addition of sintering aid, zinc oxide, carbon nanotubes, titanium carbide, and zirconium oxide improves the density and microstructure of the prepared ceramic material, thereby enhancing its strength and wear resistance. Simultaneously, the addition of zinc oxide and zirconium oxide also improves the material's antibacterial properties and compatibility. Furthermore, this invention, through a specific sintering process, can better achieve grain refinement, improving the overall performance of the prepared ceramic material.

Description

Technical Field

[0001] This invention relates to the field of medical implant technology, specifically to a medical silicon nitride ceramic material and its preparation method. Background Technology

[0002] Artificial joint replacement surgery refers to the use of materials such as metal, high molecular weight polyethylene, and ceramics to create artificial joint prostheses based on the shape, structure, and function of human joints. These prostheses are then surgically implanted into the human body to replace the function of the diseased joint, thereby relieving joint pain and restoring joint function.

[0003] Currently, knee and hip replacement are the two most common types of artificial joint replacement surgery, with a ten-year success rate exceeding 90%. Furthermore, over 80% of patients can use their implanted prostheses normally for more than 20 years, or even for life. In addition, shoulder, elbow, and ankle replacements are also continuously developing, achieving good medium- and long-term results.

[0004] Due to the inherent functional characteristics of artificial joints, friction and wear between their components, as well as the possibility of surgical instruments touching and scratching the artificial joint material during surgery, can cause certain mechanical damage to the artificial joint. Therefore, artificial joint materials need to possess certain mechanical properties and wear resistance. In addition, to better avoid inflammation after artificial joint implantation, it is particularly important for artificial joint materials to have certain antibacterial and biocompatibility properties.

[0005] In view of this, the present invention is hereby proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a medical silicon nitride ceramic material and its preparation method. The medical silicon nitride ceramic material of this invention has excellent mechanical properties and biocompatibility.

[0007] In order to achieve the above-mentioned objectives of the present invention, the following technical solution is adopted:

[0008] The first aspect of this invention provides a medical silicon nitride ceramic material, which is prepared from raw materials in the following percentages:

[0009] The composition includes 80%–86% silicon nitride powder, 6%–10% sintering aids, 1%–2% carbon nanotubes, 2%–3% nano zinc oxide, 1%–2% nano titanium carbide, and 2%–3% nano zirconium oxide.

[0010] Preferably, the medical silicon nitride ceramic material is prepared from raw materials with the following percentage contents:

[0011] The composition consists of 84% silicon nitride powder, 8% sintering aid, 1.5% carbon nanotubes, 2.5% nano zinc oxide, 1.5% titanium carbide, and 2.5% nano zirconium oxide.

[0012] Preferably, the sintering aid is selected from at least one of yttrium oxide, cerium oxide, and magnesium oxide.

[0013] Preferably, the sintering aid is a mixture of yttrium oxide and cerium oxide in a mass ratio of 1:(0.5 to 0.8).

[0014] Preferably, the particle size of the silicon nitride powder is 1–10 μm.

[0015] A second aspect of the present invention provides a method for preparing the above-mentioned medical silicon nitride ceramic material, the method comprising the following steps:

[0016] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0017] (b) The mixture is granulated and pre-pressed to obtain a preform;

[0018] (c) The preform is sintered under an inert gas atmosphere to obtain the medical silicon nitride ceramic material.

[0019] Preferably, the pre-pressing method is hot pressing or pre-sintering.

[0020] Preferably, the sintering process includes:

[0021] Heat the preform to 900-1200℃ and hold for 10-20 minutes, then continue heating to 1400-1600℃ and hold for 20-40 minutes, and finally heat to 1800-2200℃ and hold for 30-50 minutes.

[0022] Preferably, the sintering process includes:

[0023] Heat the preform to 1050℃ and hold for 15 minutes, then continue heating to 1500℃ and hold for 30 minutes, and finally heat to 2000℃ and hold for 40 minutes.

[0024] Compared with the prior art, the beneficial effects of the present invention include at least the following:

[0025] This invention, by limiting the amount of each raw material, enables the prepared medical silicon nitride ceramic material to possess excellent mechanical properties. Specifically, the addition of sintering aids, zinc oxide, carbon nanotubes, titanium carbide, and zirconium oxide improves the density and microstructure of the prepared ceramic material, thereby enhancing its strength and wear resistance. Furthermore, the addition of zinc oxide and zirconium oxide also improves the material's antibacterial properties and biocompatibility. In addition, this invention, through a specific sintering process, can better achieve grain refinement, improving the overall performance of the prepared ceramic material. Detailed Implementation

[0026] The embodiments of the technical solution of the present invention will be described in detail below with reference to the examples. The following embodiments are only used to illustrate the technical solution of the present invention more clearly, and are therefore only examples, and should not be used to limit the scope of protection of the present invention.

[0027] It should be noted that, unless otherwise stated, the technical or scientific terms used in this application should have the ordinary meaning as understood by one of ordinary skill in the art to which this invention pertains.

[0028] This invention provides a medical silicon nitride ceramic material, which is prepared from raw materials with the following percentage contents:

[0029] The composition includes 80%–88% silicon nitride powder, 6%–10% sintering aids, 1%–2% carbon nanotubes, 2%–3% nano zinc oxide, 1%–2% nano titanium carbide, and 2%–3% nano zirconium oxide.

[0030] This invention, by limiting the amount of each raw material, enables the prepared medical silicon nitride ceramic material to have excellent mechanical properties. Specifically, the addition of sintering aids, zinc oxide, carbon nanotubes, titanium carbide, and zirconium oxide improves the density and microstructure of the prepared ceramic material, thereby improving the strength and wear resistance of the ceramic material. At the same time, the addition of zinc oxide and zirconium oxide can also improve the antibacterial properties and compatibility of the material.

[0031] In one embodiment, the medical silicon nitride ceramic material is prepared from raw materials in the following percentages:

[0032] The composition consists of 84% silicon nitride powder, 8% sintering aid, 1.5% carbon nanotubes, 2.5% nano zinc oxide, 1.5% titanium carbide, and 2.5% nano zirconium oxide.

[0033] In one embodiment, the sintering aid is selected from at least one of yttrium oxide, cerium oxide, and magnesium oxide.

[0034] In one embodiment, the sintering aid is a mixture of yttrium oxide and cerium oxide in a mass ratio of 1:(0.5 to 0.8).

[0035] In one embodiment, the particle size of the silicon nitride powder is 1 to 10 μm.

[0036] Another embodiment of the present invention provides a method for preparing the above-mentioned medical silicon nitride ceramic material, the method comprising the following steps:

[0037] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0038] (b) The mixture is granulated and pre-pressed to obtain a preform;

[0039] (c) The preform is sintered under an inert gas atmosphere to obtain the medical silicon nitride ceramic material.

[0040] The present invention does not specifically limit the pre-pressing molding method. Those skilled in the art can use conventional molding methods in the field. In one embodiment, the pre-pressing molding method is hot pressing molding. In another embodiment, the pre-pressing molding method is pre-sintering molding.

[0041] In one embodiment, the sintering process includes:

[0042] Heat the preform to 900-1200℃ and hold for 10-20 minutes, then continue heating to 1400-1600℃ and hold for 20-40 minutes, and finally heat to 1800-2200℃ and hold for 30-50 minutes.

[0043] This invention, through a specific sintering process, can better achieve grain refinement and improve the overall performance of the prepared ceramic materials.

[0044] In one embodiment, the sintering process includes:

[0045] Heat the preform to 1050℃ and hold for 15 minutes, then continue heating to 1500℃ and hold for 30 minutes, and finally heat to 2000℃ and hold for 40 minutes.

[0046] The technical solution of the present invention will be further described in detail below through specific embodiments.

[0047] Example 1

[0048] This embodiment is a medical silicon nitride ceramic material, which is prepared from raw materials with the following percentage contents:

[0049] The composition consists of 80% silicon nitride powder, 10% sintering aid, 2% carbon nanotubes, 3% nano zinc oxide, 2% nano titanium carbide, and 3% nano zirconium oxide.

[0050] The sintering aid is yttrium oxide.

[0051] The particle size of the silicon nitride powder is 3 μm.

[0052] The preparation method of the above-mentioned medical silicon nitride ceramic material includes the following steps:

[0053] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0054] (b) The mixture is granulated and hot-pressed to obtain a preform;

[0055] (c) Under the protection of inert gas, the preform is heated to 900°C and held for 20 minutes, then heated to 1600°C and held for 20 minutes, and then heated to 2200°C and held for 30 minutes to obtain the medical silicon nitride ceramic material.

[0056] Example 2

[0057] This embodiment is a medical silicon nitride ceramic material, which is prepared from raw materials with the following percentage contents:

[0058] The composition consists of 88% silicon nitride powder, 6% sintering aid, 1% carbon nanotubes, 2% nano zinc oxide, 1% nano titanium carbide, and 2% nano zirconium oxide.

[0059] The sintering aid is magnesium oxide.

[0060] The particle size of the silicon nitride powder is 3 μm.

[0061] The preparation method of the above-mentioned medical silicon nitride ceramic material includes the following steps:

[0062] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0063] (b) The mixture is granulated and hot-pressed to obtain a preform;

[0064] (c) Under the protection of inert gas, the preform is heated to 1200°C and held for 10 min, then heated to 1400°C and held for 40 min, and then heated to 1800°C and held for 50 min to obtain the medical silicon nitride ceramic material.

[0065] Example 3

[0066] This embodiment is a medical silicon nitride ceramic material, which is prepared from raw materials with the following percentage contents:

[0067] The composition includes 84% ​​silicon nitride powder, 8% sintering aid, 1.5% carbon nanotubes, 2.5% nano zinc oxide, 1.5% titanium carbide, and 2.5% nano zirconium oxide.

[0068] The sintering aid is a mixture of yttrium oxide and cerium oxide in a mass ratio of 1:0.6;

[0069] The particle size of the silicon nitride powder is 3 μm.

[0070] The preparation method of the above-mentioned medical silicon nitride ceramic material includes the following steps:

[0071] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0072] (b) The mixture is granulated and hot-pressed to obtain a preform;

[0073] (c) Under the protection of inert gas, the preform is heated to 1050°C and held for 15 minutes, then heated to 1500°C and held for 30 minutes, and then heated to 2000°C and held for 40 minutes to obtain the medical silicon nitride ceramic material.

[0074] Comparative Example 1

[0075] This comparative example is a medical silicon nitride ceramic material, which is prepared from raw materials in the following percentages:

[0076] The composition includes 84% ​​silicon nitride powder, 8% sintering aid, 2.5% nano zinc oxide, 3% titanium carbide, and 2.5% nano zirconium oxide.

[0077] The sintering aid is a mixture of yttrium oxide and cerium oxide in a mass ratio of 1:0.6;

[0078] The particle size of the silicon nitride powder is 3 μm.

[0079] The preparation method of the above-mentioned medical silicon nitride ceramic material includes the following steps:

[0080] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0081] (b) The mixture is granulated and hot-pressed to obtain a preform;

[0082] (c) Under the protection of inert gas, the preform is heated to 1050°C and held for 15 minutes, then heated to 1500°C and held for 30 minutes, and then heated to 2000°C and held for 40 minutes to obtain the medical silicon nitride ceramic material.

[0083] Comparative Example 2

[0084] This comparative example is a medical silicon nitride ceramic material, which is prepared from raw materials in the following percentages:

[0085] The composition includes 84% ​​silicon nitride powder, 8% sintering aid, 3% carbon nanotubes, 2.5% nano zinc oxide, and 2.5% nano zirconium oxide.

[0086] The sintering aid is a mixture of yttrium oxide and cerium oxide in a mass ratio of 1:0.6;

[0087] The particle size of the silicon nitride powder is 3 μm.

[0088] The preparation method of the above-mentioned medical silicon nitride ceramic material includes the following steps:

[0089] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0090] (b) The mixture is granulated and hot-pressed to obtain a preform;

[0091] (c) Under the protection of inert gas, the preform is heated to 1050°C and held for 15 minutes, then heated to 1500°C and held for 30 minutes, and then heated to 2000°C and held for 40 minutes to obtain the medical silicon nitride ceramic material.

[0092] Comparative Example 3

[0093] This comparative example is a medical silicon nitride ceramic material, which is prepared from raw materials in the following percentages:

[0094] The composition includes 84% ​​silicon nitride powder, 8% sintering aid, 1.5% carbon nanotubes, 2.5% nano zinc oxide, 1.5% titanium carbide, and 2.5% nano zirconium oxide.

[0095] The sintering aid is a mixture of yttrium oxide and cerium oxide in a mass ratio of 1:0.6;

[0096] The particle size of the silicon nitride powder is 3 μm.

[0097] The preparation method of the above-mentioned medical silicon nitride ceramic material includes the following steps:

[0098] (a) Mix the raw materials according to their percentage content to obtain a mixture;

[0099] (b) The mixture is granulated and hot-pressed to obtain a preform;

[0100] (c) Under the protection of inert gas, the preform is heated to 800°C and held for 15 minutes, then heated to 1200°C and held for 30 minutes, and then heated to 2000°C and held for 40 minutes to obtain the medical silicon nitride ceramic material.

[0101] Experimental Example

[0102] Medical silicon nitride ceramic materials prepared in Example 3 and Comparative Examples 1-4 were obtained respectively;

[0103] The hardness, flexural strength, fracture toughness, and wear rate of the above-mentioned different materials were tested, and the test results are shown in Table 1:

[0104] Table 1

[0105]

[0106] As shown in Table 1:

[0107] Compared with the comparative example, the medical silicon nitride ceramic material prepared by the technical solution of this application has better mechanical properties.

[0108] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention, and they should all be covered within the scope of the claims and specification of the present invention.

Claims

1. A medical-grade silicon nitride ceramic material, characterized in that, The medical-grade silicon nitride ceramic material is prepared from the following raw materials in the following percentages: The composition includes 80%–88% silicon nitride powder, 6%–10% sintering aids, 1%–2% carbon nanotubes, 2%–3% nano zinc oxide, 1%–2% nano titanium carbide, and 2%–3% nano zirconium oxide. The preparation method of the medical silicon nitride ceramic material includes the following steps: (a) Mix the raw materials according to their percentage content to obtain a mixture; (b) The mixture is granulated and pre-pressed to obtain a preform; (c) The preform is sintered under an inert gas atmosphere to obtain the medical silicon nitride ceramic material. The sintering process includes: Heat the preform to 900~1200℃ and hold for 10~20 minutes, then continue heating to 1400~1600℃ and hold for 20~40 minutes, and then heat to 1800~2200℃ and hold for 30~50 minutes.

2. The medical silicon nitride ceramic material according to claim 1, characterized in that, The medical-grade silicon nitride ceramic material is prepared from the following raw materials in the following percentages: The composition consists of 84% silicon nitride powder, 8% sintering aid, 1.5% carbon nanotubes, 2.5% nano zinc oxide, 1.5% nano titanium carbide, and 2.5% nano zirconium oxide.

3. The medical silicon nitride ceramic material according to claim 1 or 2, characterized in that, The sintering aid is selected from at least one of yttrium oxide, cerium oxide, and magnesium oxide.

4. The medical silicon nitride ceramic material according to claim 1, characterized in that, The sintering aid is a mixture of yttrium oxide and cerium oxide in a mass ratio of 1:(0.5~0.8).

5. The medical silicon nitride ceramic material according to claim 1, characterized in that, The particle size of the silicon nitride powder is 1~10μm.

6. The medical silicon nitride ceramic material according to claim 1, characterized in that, The sintering process includes: Heat the preform to 1050℃ and hold for 15 minutes, then continue heating to 1500℃ and hold for 30 minutes, and finally heat to 2000℃ and hold for 40 minutes.

Images