An artificial bone material and a method for producing the same
By using a hot-pressing and sintering process involving bioceramic mixed powder and wax materials, the problem of insufficient forming precision in ceramic bones was solved, enabling the preparation of high-precision ceramic bones, reducing processing costs, and ensuring biocompatibility and mechanical properties.
Patent Information
- Application Number
- CN202310513618.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-09
- Publication Date
- 2025-11-21
- Estimated Expiration
- 2043-05-09
AI Technical Summary
Existing technologies cannot produce ceramic skeletons with the required dimensional accuracy. High-precision processing is required after molding, which is difficult and costly.
Bioceramic wax slurry was prepared by mixing bioceramic powder, fully refined paraffin wax, beeswax, and oleic acid. Artificial bone material was prepared by hot pressing, wax removal, glue removal, and gas pressure sintering. Deformation during the molding and sintering process was controlled to ensure dimensional accuracy.
Ceramic bone with high dimensional accuracy can be prepared without high-precision processing, reducing costs. It is suitable for complex and irregular bone structures, and produces no byproducts in the human body. It also has good biocompatibility and mechanical strength.
Abstract
Description
Technical Field
[0001] This invention relates to the field of artificial bone technology, and more specifically, to an artificial bone material and its preparation method. Background Technology
[0002] Repair and reconstruction due to injuries and defects has always been a challenge in biomedicine, and artificial bone materials play a crucial role in this process. Artificial bones typically include metal bone, polymer bone, and ceramic bone. Metal bone, after long-term corrosion within the body, releases metal ion byproducts, which can seriously harm the nervous and endocrine systems. Polymer bone has lower mechanical properties and is prone to stress relaxation and creep. Ceramic bone, with its excellent biocompatibility, has become a more ideal artificial bone defect repair material after metal and polymer bone. However, the structural complexity of bones varies in different parts of the body. For bone structures of different shapes, especially complex and irregular bone structures, current technology struggles to produce ceramic bone with the required dimensional accuracy. High-precision machining after molding is usually necessary before use. However, the high brittleness of ceramics makes them unable to withstand the forces during machining, resulting in difficult processing, high costs, and difficulty in producing suitable artificial bone. Summary of the Invention
[0003] This invention provides an artificial bone material and its preparation method to solve the problems that the dimensional accuracy of ceramic bones formed by existing technologies cannot meet the requirements for use, and that high-precision processing is required after forming, which is difficult and costly to produce artificial bones that meet the requirements.
[0004] On one hand, the present invention provides a method for preparing artificial bone material, comprising the following steps: mixing bioceramic mixed powder, fully refined paraffin wax, beeswax and oleic acid to obtain a fluid bioceramic wax slurry; injecting the bioceramic wax slurry into an artificial bone mold by hot pressing, and demolding after molding to obtain an artificial bone wax blank; embedding the artificial bone wax blank in an active adsorbent and removing the wax to obtain an artificial bone preform; subjecting the artificial bone preform to glue removal treatment and gas pressure sintering in sequence to obtain the artificial bone material.
[0005] In some embodiments of the present invention, the bioceramic mixed powder comprises 85-90 parts by weight, the fully refined paraffin comprises 9-14 parts, the beeswax comprises 0.5-1.5 parts, and the oleic acid comprises 0.5-1 parts.
[0006] In some embodiments of the present invention, the bioceramic mixed powder comprises bioceramic powder and a biocompatible zinc-containing powder; the weight ratio of the zinc-containing powder to the bioceramic powder is (15-30):(70-85).
[0007] In some embodiments of the present invention, the zinc-containing powder includes one or more of zinc oxide, zinc carbonate, and zinc sphalerite powder, and the bioceramic powder includes silicon nitride ceramic powder with added sintering aids, wherein the weight ratio of the sintering aids to the silicon nitride ceramic powder is (5-15):(85-95). Preferably, the sintering aids include one or more of alumina, yttrium oxide, ytterbium oxide, magnesium oxide, and lanthanum oxide.
[0008] In some embodiments of the present invention, bioceramic mixed powder, fully refined paraffin wax, beeswax and oleic acid are stirred and mixed at a temperature of 70-80°C to obtain a fluid bioceramic wax slurry.
[0009] In some embodiments of the present invention, the specific process of hot-press casting artificial bone wax blank includes: injecting the bioceramic wax slurry into an artificial bone mold at a molding pressure of not less than 0.5 MPa and a molding temperature of 65-70°C, and demolding to obtain the artificial bone wax blank.
[0010] In some embodiments of the present invention, the active adsorbent is active alumina powder; the dewaxing temperature for dewaxing the artificial bone wax blank is 220-250°C, and the dewaxing time is 30-50 hours.
[0011] In some embodiments of the present invention, the glue removal process includes: heating to 550-650°C at a heating rate of 15-20°C / h and holding at that temperature for 2-4 hours to complete the glue removal.
[0012] In some embodiments of the present invention, the gas pressure sintering includes a first sintering and a second sintering performed sequentially; the first sintering is: heating to 1450°C at a heating rate of 180-240°C / h under a pressure of 3-5 MPa and holding at that temperature for 1-3 hours; the second sintering is: heating to 1620-1680°C at a heating rate of 150-180°C / h under a pressure of 5-10 MPa and holding at that temperature for 2-4 hours.
[0013] On the other hand, the present invention also provides an artificial bone material, which is prepared according to any one of the above preparation methods.
[0014] Compared with the prior art, the present invention has the following beneficial effects:
[0015] (1) This invention uses 85-90 parts of bioceramic mixed powder, 9-14 parts of fully refined paraffin wax, 0.5-1.5 parts of beeswax, and 0.5-1 parts of oleic acid as raw materials to prepare bioceramic wax slurry. The fully refined paraffin wax has low oil content, few impurities, and good plasticity. As a binder, it works in conjunction with beeswax as a surfactant, reducing the content of fully refined paraffin wax and improving the performance of the molded product. Oleic acid acts as a dispersant, adjusting the viscosity and suspension of the wax slurry. Based on this, it is molded by hot pressing at a molding pressure of not less than 0.5 MPa and a molding temperature of 65-70°C. The resulting artificial bone wax blank has high dimensional accuracy. Under the wax removal, glue removal, and air pressure sintering designed in this invention, wax removal, glue removal, and... The deformation during the gas pressure sintering process maintains dimensional accuracy while achieving good mechanical strength. The finished product obtained after wax removal, glue removal, and gas pressure sintering has high dimensional accuracy and meets usage requirements. It eliminates the need for high-precision processing, avoiding the problems caused by the high brittleness of ceramics, which makes it difficult to withstand the forces during processing and thus difficult to produce qualified artificial bones. The cost is low. The preparation method of this invention can be used to prepare bone shapes of arbitrary structures, especially suitable for complex and irregular bone structures, without the need for processing, saving time and processing costs. When the product produced by this invention is used in the human body, no useless byproducts are generated, and there are no negative effects. It has the characteristics of high quality and few impurities, and has high economic efficiency and feasibility.
[0016] (2) The bioceramic mixed powder of the present invention includes bioceramic powder and zinc-containing powder with biocompatibility. Zinc promotes osteogenesis and bone growth. At the same time, the bioceramic powder and zinc-containing powder work together to improve the mechanical strength of artificial bone. The zinc-containing powder includes one or more of zinc oxide, zinc carbonate, and zinc sphalerite powder. The bioceramic powder includes silicon nitride ceramic powder with added sintering aid. It has excellent biocompatibility and will not produce side effects after implantation into the human body. It is beneficial to maintain the normal physiological environment of the human body and promote bone growth. The weight ratio of sintering aid to silicon nitride ceramic powder is (5-15):(85-95). While promoting sintering, it ensures the content of silicon nitride ceramic powder, thereby ensuring the strength of the product. The weight ratio of zinc-containing powder to bioceramic powder is (15-30):(70-85). Under this ratio, the zinc content of the bioceramic mixed powder can effectively ensure the release of a reasonable amount of zinc ions. In addition, the bioceramic powder plays the main role in enhancing mechanical strength, and an appropriate amount of zinc acts as a reinforcing phase, dispersed between the bioceramic powders, further enhancing mechanical strength.
[0017] (3) In this invention, bioceramic mixed powder, fully refined paraffin wax, beeswax, and oleic acid are stirred and mixed at a temperature of 70-80°C. The wax melts without deteriorating and has excellent fluidity, promoting thorough mixing of the bioceramic mixed powder in the fully refined paraffin wax, beeswax, and oleic acid. The bioceramic wax slurry is a fluid with good fluidity, uniform composition, and does not deteriorate. It can form a fluid at low temperatures, has a small molecular weight, and few molding defects, providing a prerequisite for effective control of deformation and ensuring dimensional accuracy. Based on the bioceramic wax slurry with good fluidity that can be obtained at low temperatures in this invention, the bioceramic wax slurry is injected into an artificial bone mold in a fluid form. Hot pressing is performed at a molding pressure of not less than 0.5 MPa and a molding temperature of 65-70°C. The fluid fully fills all positions of the artificial bone mold, resulting in artificial bone wax blanks with very few defects and high dimensional accuracy.
[0018] (4) In this invention, activated alumina powder is used as an active adsorbent to dewax artificial bone wax blanks at a dewaxing temperature of 220-250℃ for 30-50 hours. This dewaxing temperature allows the wax to be discharged at a reasonable rate, avoiding excessively slow dewaxing speed leading to a long production cycle and excessively fast dewaxing speed leading to product deformation and affecting dimensional accuracy. Using activated alumina powder as an active adsorbent is beneficial in two ways: firstly, it helps to adsorb the discharged wax in a timely manner in accordance with the dewaxing temperature; secondly, during the dewaxing process of artificial bone wax blanks, activated alumina penetrates from the dewaxing channels of artificial bone wax blanks, bridging and connecting in the gaps left by dewaxing to form a skeleton. Combined with bioceramic powder, it enhances structural stability and further maintains dimensional accuracy.
[0019] (5) The present invention heats the temperature to 550-650℃ at a heating rate of 15-20℃ / h and then holds it for 2-4 hours to complete the glue removal. The design of the heating rate, temperature and holding time fully considers the design of each component and its dosage in the present invention. The designed glue removal process enables the present invention to remove glue at a reasonable speed, avoiding the production cycle being too long due to the glue removal speed being too slow and the product deformation being affected by the glue removal speed being too fast, thus affecting the dimensional accuracy. This invention relates to a gas pressure sintering process comprising primary sintering and secondary sintering. Under a pressure of 3-5 MPa, the temperature is raised to 1450°C at a rate of 180-240°C / h and held for 1-3 hours. A liquid phase forms at the silicon nitride grain boundaries, and the α-Si3N4 phase begins to transform into β-Si3N4, completing the primary sintering for crystal pre-growth. Under a pressure of 5-10 MPa, the temperature is raised to 1620-1680°C at a rate of 150-180°C / h and held for 2-4 hours. The α / β phase transformation is enhanced, the relative content of the β-Si3N4 phase increases significantly, and the α-Si3N4 phase completely disappears, with β-Si3N4 becoming the dominant crystalline phase. This completes the phase transformation and the secondary sintering process. This process ensures mechanical strength while maintaining dimensional accuracy, and simultaneously meets the porosity requirements of artificial bone. Detailed Implementation
[0020] To make the objectives, technical solutions and advantages of the present invention clearer, the various aspects of the present invention will be described in detail below with reference to specific embodiments. However, these specific embodiments are only used to illustrate the present invention and do not constitute any limitation on the scope of protection and the substantive content of the present invention.
[0021] This invention provides a method for preparing artificial bone material, comprising the following steps:
[0022] By weight, 85-90 parts of bioceramic mixed powder, 9-14 parts of fully refined paraffin wax, 0.5-1.5 parts of beeswax, and 0.5-1 parts of oleic acid are thoroughly mixed at a temperature of 70-80°C to obtain a fluid bioceramic wax slurry. The bioceramic mixed powder comprises bioceramic powder and biocompatible zinc-containing powder, with a weight ratio of zinc-containing powder to bioceramic powder of (15-30):(70-85). The zinc-containing powder includes one or more of zinc oxide, zinc carbonate, and zinc sphalerite powder. The bioceramic powder includes silicon nitride ceramic powder with added sintering aids, with a weight ratio of sintering aids to silicon nitride ceramic powder of (5-15):(85-95). Preferably, the sintering aids include one or more of alumina, yttrium oxide, ytterbium oxide, magnesium oxide, and lanthanum oxide.
[0023] Bioceramic wax slurry is injected into an artificial bone mold by hot pressing at a molding pressure of not less than 0.5 MPa and a molding temperature of 65-70℃. After molding, the mold is demolded to obtain an artificial bone wax blank.
[0024] Artificial bone wax blanks are embedded in an active adsorbent and dewaxing is carried out at a dewaxing temperature of 220-250℃ and a dewaxing time of 30-50 hours to obtain artificial bone blanks; wherein, the active adsorbent is active alumina powder.
[0025] The artificial bone preform is subjected to debinding and gas pressure sintering in sequence to obtain artificial bone material. The debinding process includes heating to 550-650℃ at a heating rate of 15-20℃ / h and holding for 2-4 hours to complete the debinding. The gas pressure sintering includes a first sintering and a second sintering in sequence. The first sintering is carried out by heating to 1450℃ at a heating rate of 180-240℃ / h under a pressure of 3-5MPa and holding for 1-3 hours. The second sintering is carried out by heating to 1620-1680℃ at a heating rate of 150-180℃ / h under a pressure of 5-10MPa and holding for 2-4 hours.
[0026] The present invention also provides an artificial bone material, which is prepared according to the preparation method of the present invention.
[0027] Example 1:
[0028] This embodiment provides a method for preparing artificial bone material, including the following steps:
[0029] Preparation of bioceramic mixed powder: Bioceramic powder and biocompatible zinc-containing powder are thoroughly mixed using a mixer to obtain bioceramic mixed powder; wherein the weight ratio of zinc-containing powder to bioceramic powder is 15:70, the zinc-containing powder includes zinc oxide, zinc carbonate, and zinc sphalerite powder, and the bioceramic powder includes silicon nitride ceramic powder with added sintering aids, the weight ratio of sintering aids to silicon nitride ceramic powder is 5:85. Preferably, the sintering aids include one or more of alumina, yttrium oxide, ytterbium oxide, magnesium oxide, and lanthanum oxide.
[0030] Preparation of bioceramic wax slurry: By weight, 85 parts of bioceramic mixed powder, 9 parts of fully refined paraffin wax, 0.5 parts of beeswax, and 0.5 parts of oleic acid are added to a heated mixer and kept at 70°C. The mixture is stirred thoroughly until melted and homogeneous to obtain a fluid bioceramic wax slurry.
[0031] Preparation of artificial bone wax blank: Bioceramic wax slurry was injected into an artificial bone metal mold by hot pressing at a molding pressure of 0.5 MPa and a molding temperature of 65°C. After demolding, the artificial bone wax blank was obtained.
[0032] Preparation of artificial bone preform: The artificial bone wax preform is completely embedded in an active adsorbent (active alumina powder) and placed in an oven at a wax removal temperature of 220°C for 50 hours to fully remove wax, thus obtaining the artificial bone preform. In this embodiment, the amount of active adsorbent is not limited, as long as the artificial bone wax preform is completely embedded in the active adsorbent. The active adsorbent is beneficial for timely adsorption of the wax removed in conjunction with the wax removal temperature. On the other hand, during the wax removal process of the artificial bone wax preform, the active alumina seeps in from the wax removal channels of the artificial bone wax preform, bridging and connecting in the gaps left by wax removal to form a framework. Combined with bioceramic powder, this enhances structural stability and further maintains dimensional accuracy.
[0033] Preparation of artificial bone blank: The artificial bone blank is subjected to debinding treatment. Specifically, the artificial bone blank is placed in a muffle furnace and heated to 550°C at a heating rate of 15°C / h, and then held at that temperature for 4 hours to complete the debinding and obtain the artificial bone blank.
[0034] Preparation of finished artificial bone: The artificial bone blank is placed in an atmosphere pressure sintering furnace for gas pressure sintering. Gas pressure sintering includes a first sintering and a second sintering performed sequentially. Specifically, under a pressure of 3 MPa, the temperature is raised to 1450°C at a heating rate of 180°C / h and held for 1 hour to complete the first sintering for crystal pre-growth; under a pressure of 5 MPa, the temperature is raised to 1620°C at a heating rate of 150°C / h and held for 4 hours to achieve complete phase transformation and complete the second sintering, resulting in a high-quality artificial bone material.
[0035] This embodiment also provides an artificial bone material, which is prepared according to the preparation method of this embodiment. The artificial bone material prepared by the preparation method of this embodiment has excellent mechanical strength, and its porosity is similar to that of human bone, both of which meet the requirements for use in the human body environment. In addition, the artificial bone material has high dimensional accuracy, meets the requirements for use, and does not require high-precision processing. This avoids the processing difficulties caused by the high brittleness of ceramics (unable to withstand the forces during processing), thus making it difficult to process artificial bone that meets the requirements. The cost is also low.
[0036] Example 2:
[0037] This embodiment provides a method for preparing artificial bone material, including the following steps:
[0038] Preparation of bioceramic mixed powder: Bioceramic powder and biocompatible zinc-containing powder are thoroughly mixed using a mixer to obtain bioceramic mixed powder; wherein the weight ratio of zinc-containing powder to bioceramic powder is 20:75, the zinc-containing powder includes zinc oxide and zinc carbonate, and the bioceramic powder includes silicon nitride ceramic powder with added sintering aids, the weight ratio of sintering aids to silicon nitride ceramic powder is 8:87. Preferably, the sintering aids include one or more of alumina, yttrium oxide, ytterbium oxide, magnesium oxide, and lanthanum oxide.
[0039] Preparation of bioceramic wax slurry: By weight, 87 parts of bioceramic mixed powder, 11 parts of fully refined paraffin wax, 0.8 parts of beeswax and 0.7 parts of oleic acid were added to a heated mixer and kept at 73°C. The mixture was stirred and mixed thoroughly until it melted and homogeneous to obtain a fluid bioceramic wax slurry.
[0040] Preparation of artificial bone wax blank: Bioceramic wax slurry was injected into an artificial bone metal mold by hot pressing at a molding pressure of 0.8 MPa and a molding temperature of 67°C. After demolding, the artificial bone wax blank was obtained.
[0041] Preparation of artificial bone preform: The artificial bone wax preform is completely embedded in an active adsorbent (active alumina powder) and placed in an oven at a wax removal temperature of 230°C for 45 hours to fully remove wax, thus obtaining the artificial bone preform. In this embodiment, the amount of active adsorbent is not limited, as long as the artificial bone wax preform is completely embedded in the active adsorbent. The active adsorbent is beneficial in two ways: firstly, it helps to adsorb the wax removed in a timely manner in conjunction with the wax removal temperature; secondly, during the wax removal process of the artificial bone wax preform, the active alumina seeps in from the wax removal channels of the artificial bone wax preform, bridging and connecting in the gaps left by wax removal to form a framework. Combined with bioceramic powder, this enhances structural stability and further maintains dimensional accuracy.
[0042] Preparation of artificial bone blank: The artificial bone blank is subjected to debinding treatment. Specifically, the artificial bone blank is placed in a muffle furnace and heated to 580°C at a heating rate of 17°C / h, and then held at that temperature for 3 hours to complete the debinding and obtain the artificial bone blank.
[0043] Preparation of finished artificial bone: The artificial bone blank is placed in an atmosphere pressure sintering furnace for gas pressure sintering. Gas pressure sintering includes a first sintering and a second sintering performed sequentially. Specifically, under a pressure of 4 MPa, the temperature is raised to 1450°C at a heating rate of 200°C / h and held for 2 hours to complete the first sintering for crystal pre-growth; under a pressure of 7 MPa, the temperature is raised to 1650°C at a heating rate of 160°C / h and held for 3.5 hours to achieve complete phase transformation and complete the second sintering, resulting in a high-quality artificial bone material.
[0044] This embodiment also provides an artificial bone material, which is prepared according to the preparation method of this embodiment. The artificial bone material prepared by the preparation method of this embodiment has excellent mechanical strength, and its porosity is similar to that of human bone, both of which meet the requirements for use in the human body environment. In addition, the artificial bone material has high dimensional accuracy, meets the requirements for use, and does not require high-precision processing. This avoids the processing difficulties caused by the high brittleness of ceramics (unable to withstand the forces during processing), thus making it difficult to process artificial bone that meets the requirements. The cost is also low.
[0045] Example 3:
[0046] This embodiment provides a method for preparing artificial bone material, including the following steps:
[0047] Preparation of bioceramic mixed powder: Bioceramic powder and biocompatible zinc-containing powder are thoroughly mixed using a mixer to obtain bioceramic mixed powder; wherein the weight ratio of zinc-containing powder to bioceramic powder is 25:80, the zinc-containing powder includes zinc oxide, and the bioceramic powder includes silicon nitride ceramic powder with added sintering aids, the weight ratio of sintering aids to silicon nitride ceramic powder is 11:92. Preferably, the sintering aids include one or more of alumina, yttrium oxide, ytterbium oxide, magnesium oxide, and lanthanum oxide.
[0048] Preparation of bioceramic wax slurry: By weight, 88 parts of bioceramic mixed powder, 13 parts of fully refined paraffin wax, 1.2 parts of beeswax and 0.8 parts of oleic acid were added to a heated mixer and kept at 77°C. The mixture was stirred and mixed thoroughly until it melted and homogeneous to obtain a fluid bioceramic wax slurry.
[0049] Preparation of artificial bone wax blank: Bioceramic wax slurry was injected into an artificial bone metal mold by hot pressing at a molding pressure of 1 MPa and a molding temperature of 69°C. After demolding, the artificial bone wax blank was obtained.
[0050] Preparation of artificial bone preform: The artificial bone wax preform is completely embedded in an active adsorbent (activated alumina powder) and placed in an oven at a wax removal temperature of 240°C for 40 hours to fully remove wax, thus obtaining the artificial bone preform. In this embodiment, the amount of active adsorbent is not limited, as long as the artificial bone wax preform is completely embedded in the active adsorbent. The active adsorbent is beneficial in two ways: firstly, it helps to adsorb the wax removed in a timely manner in conjunction with the wax removal temperature; secondly, during the wax removal process of the artificial bone wax preform, activated alumina seeps in from the wax removal channels of the artificial bone wax preform, bridging and connecting in the gaps left by wax removal to form a framework. Combined with bioceramic powder, this enhances structural stability and further maintains dimensional accuracy.
[0051] Preparation of artificial bone blank: The artificial bone blank is subjected to debinding treatment. Specifically, the artificial bone blank is placed in a muffle furnace and heated to 620°C at a heating rate of 19°C / h, and then held at that temperature for 2.5 hours to complete the debinding and obtain the artificial bone blank.
[0052] Preparation of finished artificial bone: The artificial bone blank is placed in an atmosphere pressure sintering furnace for gas pressure sintering. Gas pressure sintering includes a first sintering and a second sintering performed sequentially. Specifically, under a pressure of 4.5 MPa, the temperature is raised to 1450 °C at a heating rate of 220 °C / h and held for 2.5 hours to complete the first sintering for crystal pre-growth; under a pressure of 8 MPa, the temperature is raised to 1670 °C at a heating rate of 170 °C / h and held for 3 hours to achieve complete phase transformation and complete the second sintering, resulting in a high-quality artificial bone material.
[0053] This embodiment also provides an artificial bone material, which is prepared according to the preparation method of this embodiment. The artificial bone material prepared by the preparation method of this embodiment has excellent mechanical strength, and its porosity is similar to that of human bone, both of which meet the requirements for use in the human body environment. In addition, the artificial bone material has high dimensional accuracy, meets the requirements for use, and does not require high-precision processing. This avoids the processing difficulties caused by the high brittleness of ceramics (unable to withstand the forces during processing), thus making it difficult to process artificial bone that meets the requirements. The cost is also low.
[0054] Example 4:
[0055] This embodiment provides a method for preparing artificial bone material, including the following steps:
[0056] Preparation of bioceramic mixed powder: Bioceramic powder and biocompatible zinc-containing powder are thoroughly mixed using a mixer to obtain bioceramic mixed powder; wherein the weight ratio of zinc-containing powder to bioceramic powder is 30:85, the zinc-containing powder includes zinc carbonate, and the bioceramic powder includes silicon nitride ceramic powder with added sintering aids, the weight ratio of sintering aids to silicon nitride ceramic powder is 15:95. Preferably, the sintering aids include one or more of alumina, yttrium oxide, ytterbium oxide, magnesium oxide, and lanthanum oxide.
[0057] Preparation of bioceramic wax slurry: By weight, 90 parts of bioceramic mixed powder, 14 parts of fully refined paraffin wax, 1.5 parts of beeswax and 1 part of oleic acid are added to a heated mixer, and the temperature is maintained at 80°C. The mixture is stirred and mixed thoroughly until it melts and becomes uniform, thus obtaining a fluid bioceramic wax slurry.
[0058] Preparation of artificial bone wax blank: Bioceramic wax slurry was injected into an artificial bone metal mold by hot press casting at a molding pressure of 1.2 MPa and a molding temperature of 70°C. After demolding, the artificial bone wax blank was obtained.
[0059] Preparation of artificial bone preform: The artificial bone wax preform is completely embedded in an active adsorbent (active alumina powder) and placed in an oven at a wax removal temperature of 250°C for 30 hours to fully remove wax, thus obtaining the artificial bone preform. In this embodiment, the amount of active adsorbent is not limited, as long as the artificial bone wax preform is completely embedded in the active adsorbent. The active adsorbent is beneficial for timely adsorption of the wax removed in conjunction with the wax removal temperature. On the other hand, during the wax removal process of the artificial bone wax preform, the active alumina seeps in from the wax removal channels of the artificial bone wax preform, bridging and connecting in the gaps left by wax removal to form a framework. Combined with bioceramic powder, this enhances structural stability and further maintains dimensional accuracy.
[0060] Preparation of artificial bone blank: The artificial bone blank is subjected to debinding treatment. Specifically, the artificial bone blank is placed in a muffle furnace and heated to 650°C at a heating rate of 20°C / h, and then held at that temperature for 2 hours to complete the debinding and obtain the artificial bone blank.
[0061] Preparation of finished artificial bone: The artificial bone blank is placed in an atmosphere pressure sintering furnace for gas pressure sintering. Gas pressure sintering includes a first sintering and a second sintering performed sequentially. Specifically, under a pressure of 5 MPa, the temperature is raised to 1450°C at a heating rate of 240°C / h and held for 3 hours to complete the first sintering for crystal pre-growth; under a pressure of 10 MPa, the temperature is raised to 1680°C at a heating rate of 180°C / h and held for 2 hours to achieve complete phase transformation and complete the second sintering, resulting in a high-quality artificial bone material.
[0062] This embodiment also provides an artificial bone material, which is prepared according to the preparation method of this embodiment. The artificial bone material prepared by the preparation method of this embodiment has excellent mechanical strength, and its porosity is similar to that of human bone, both of which meet the requirements for use in the human body environment. In addition, the artificial bone material has high dimensional accuracy, meets the requirements for use, and does not require high-precision processing. This avoids the processing difficulties caused by the high brittleness of ceramics (unable to withstand the forces during processing), thus making it difficult to process artificial bone that meets the requirements. The cost is also low.
[0063] The present invention has been described above with reference to specific embodiments. These specific embodiments are merely exemplary and should not be construed as limiting the scope of protection of the present invention. Those skilled in the art can make various modifications, changes, or substitutions without departing from the essence of the present invention. Therefore, various equivalent variations made according to the present invention still fall within the scope of the present invention.
Claims
1. A method for preparing an artificial bone material, characterized in that, Includes the following steps: A mixture of bioceramic powder, fully refined paraffin wax, beeswax, and oleic acid is prepared to obtain a fluid bioceramic wax slurry. The bioceramic powder includes bioceramic powder and a zinc-containing powder with biocompatibility. The bioceramic powder includes silicon nitride ceramic powder with added sintering aids. The bioceramic wax slurry is injected into an artificial bone mold by hot pressing, and after molding, it is demolded to obtain an artificial bone wax blank. The artificial bone wax blank is embedded in an active adsorbent and the wax is removed to obtain an artificial bone material blank. The active adsorbent is active alumina powder. The wax removal temperature of the artificial bone wax blank is 220-250℃ and the wax removal time is 30-50 hours. The artificial bone preform is subjected to debinding treatment and gas pressure sintering in sequence to obtain the artificial bone material. The debinding treatment includes heating to 550-650℃ at a heating rate of 15-20℃ / h and holding at that temperature for 2-4 hours to complete the debinding. The gas pressure sintering includes a first sintering and a second sintering performed sequentially. The first sintering is performed by heating to 1450°C at a heating rate of 180-240°C / h under a pressure of 3-5 MPa and holding at that temperature for 1-3 hours. The second sintering is performed by heating to 1620-1680°C at a heating rate of 150-180°C / h under a pressure of 5-10 MPa and holding at that temperature for 2-4 hours.
2. The method for preparing artificial bone material as described in claim 1, characterized in that, By weight, the bioceramic mixed powder comprises 85-90 parts, the fully refined paraffin wax comprises 9-14 parts, the beeswax comprises 0.5-1.5 parts, and the oleic acid comprises 0.5-1 parts.
3. The method for preparing artificial bone material as described in claim 1, characterized in that, The weight ratio of the zinc-containing powder to the bioceramic powder is (15-30):(70-85).
4. The method for preparing artificial bone material as described in claim 3, characterized in that, The zinc-containing powder includes one or more of zinc oxide, zinc carbonate, and zinc sphalerite powder, and the weight ratio of the sintering aid to the silicon nitride ceramic powder is (5-15):(85-95).
5. The method for preparing artificial bone material as described in claim 1, characterized in that, Bioceramic powder, fully refined paraffin wax, beeswax, and oleic acid are stirred and mixed at a temperature of 70-80℃ to obtain a fluid bioceramic wax slurry.
6. The method for preparing artificial bone material according to claim 1, characterized in that, The specific process of hot-press casting artificial bone wax blank includes: injecting the bioceramic wax slurry into the artificial bone mold at a molding pressure of not less than 0.5 MPa and a molding temperature of 65-70°C, and demolding to obtain the artificial bone wax blank.
7. An artificial bone material, characterized in that, The artificial bone material is prepared by the method according to any one of claims 1-6.
Citation Information
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Preparation method of three-dimensional network ceramic framework
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