CN111875408A - Preparation method of hydroxyapatite porous ceramic capable of being used as artificial bone - Google Patents
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Abstract
The invention belongs to the technical field of bioengineering and material science, and particularly relates to a preparation method of hydroxyapatite porous ceramic used as artificial bone. The preparation process can be realized by the following steps: taking deionized water, a dispersing agent, a binder, hydroxyapatite ceramic powder and a pore-forming agent as initial raw materials, and carrying out ball milling and mixing to obtain slurry with stable dispersion; drying the obtained slurry in a rotary evaporator, and sieving for later use; performing mechanical pressing on the sieved powder, demolding, and drying in an oven; and sintering the dried blank in an air atmosphere furnace to obtain the hydroxyapatite porous ceramic. The material prepared by the invention has reliable performance, and has the characteristics of simple process, easy large-scale production and the like.
Description
Technical Field
The invention belongs to the technical field of bioengineering and material science, and particularly relates to a preparation method of hydroxyapatite porous ceramic used as artificial bone.
Background
Bone defects are common clinical cases, and human bone transplantation is a common rehabilitation strategy. The commonly used repair materials at present comprise autogenous bone, allogeneic bone and artificial synthetic materials, and the materials all have certain defects. The autologous bone has no immunological rejection reaction, has good repairing effect, but has limited material selection; the allogeneic bone has wide material sources, but the immunologic rejection reaction is easily caused, and the repairing effect is poor; in recent years, research and application of synthetic materials have been greatly advanced, and a feasible method is provided for repairing bone defects. At present, the artificially synthesized materials comprise polymer high molecular materials, titanium alloy materials, biodegradable ceramics and the like, wherein the biodegradable ceramics comprise tricalcium phosphate, hydroxyapatite and the like, the biodegradable ceramics have mineral compositions similar to human bones, elements such as calcium, phosphorus and the like in the compositions can be replaced through normal metabolic pathways of human bodies, and hydroxyl groups capable of generating bonding action with human tissues are also contained, so the artificially synthesized materials have good bioactivity and biocompatibility.
The traditional ceramic materials such as tricalcium phosphate, hydroxyapatite and the like have no air holes inside or have small pore diameter of the air holes, so that pore channels cannot meet the structural requirement of the inward growth of bone units, the nutrition delivery and the induced growth of bones are influenced, and the clinical application is limited to a certain extent. When the ceramic material systems are subjected to pore design, the application of the materials is often influenced because the mechanical strength and the toughness of the materials are greatly reduced.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of hydroxyapatite porous ceramic used as artificial bone.
The invention adopts the following technical scheme for achieving the purpose:
a method for preparing hydroxyapatite porous ceramics used as artificial bones comprises the steps of mixing materials, preparing a green body and sintering the green body; the specific process steps are as follows:
1) mixing materials: taking deionized water, a dispersing agent, a binder, hydroxyapatite ceramic powder and a pore-forming agent as initial raw materials, and carrying out ball milling and mixing to obtain slurry with stable dispersion; drying the obtained slurry in a rotary evaporator, and sieving for later use; the adding amount of the deionized water is 1-3 times of the mass of the hydroxyapatite ceramic powder; the addition amount of the dispersing agent is 0.5-1.0% of the mass of the hydroxyapatite ceramic powder; the addition amount of the binder is 1.0-4.0% of the mass of the ceramic powder; the hydroxyapatite ceramic powder has the purity of more than 99.5 percent and the average particle size of 0.1-2.0 mu m; the addition amount of the pore-forming agent is 10-40% of the mass of the hydroxyapatite ceramic powder;
2) preparing a blank body: performing mechanical pressing on the sieved powder, demolding, and drying in an oven;
3) sintering of the green body: and sintering the dried blank in an air atmosphere furnace to obtain the hydroxyapatite porous ceramic.
The dispersant is one of ammonium polyacrylate and polyacrylamide.
The binder is one of polyvinyl alcohol and polyethylene glycol.
The pore-forming agent is one or a mixture of more of starch, activated carbon powder and polymethyl methacrylate microspheres.
Performing ball milling and mixing, wherein zirconia balls are used as a ball milling medium, and the ball material ratio is 2: 1-4: 1; the ball milling speed is 100-500 r/min, and the ball milling time is 6-12 h; the screening mesh number is 60-325 meshes.
The pressure of the machine pressing is 30-200 MPa; the temperature in the drying process is 100-150 ℃, and the heat preservation time is 0.5-5 h.
The sintering process is to preserve heat for 2-5 hours at 1000-1300 ℃.
The invention provides a preparation method of hydroxyapatite porous ceramic capable of being used as artificial bone, which takes hydroxyapatite ceramic powder as a main raw material, and obtains the hydroxyapatite porous ceramic material with certain porosity and mechanical property meeting the clinical use requirement by a pore-forming mechanism of adding pore-forming agent and combining a mechanical pressing forming and pressureless sintering process; the material prepared by the method has reliable performance, and has the characteristics of simple process, easy large-scale production and the like.
Detailed Description
The invention is illustrated by the following examples:
example 1:
weighing 100g of hydroxyapatite ceramic powder with the average particle size of 0.1 mu m, 300g of deionized water, 1.0g of polyacrylamide, 1.0g of polyvinyl alcohol and 40g of starch, taking zirconia balls as a ball milling medium, mixing the materials at a ball-to-material ratio of 4:1 and a rotating speed of 300r/min for 8 hours; the obtained slurry is filtered by a 60-mesh sieve after rotary evaporation, and the powder is molded by mechanical pressing under the pressure of 30 MPa; keeping the demoulded blank in an oven at 100 ℃ for 5 hours; placing the dried blank in a high-temperature sintering furnace, and keeping the temperature for 4 hours at 1000 ℃; the porosity of the prepared hydroxyapatite porous ceramic is 43.8%, and the compressive strength is 6.8 MPa.
Example 2:
weighing 100g of hydroxyapatite ceramic powder with the average particle size of 0.5 mu m, 200g of deionized water, 0.7g of polyacrylamide, 3.0g of polyethylene glycol, 15g of activated carbon powder and 5g of starch, taking zirconia balls as a ball milling medium, mixing the materials at a ball-to-ball ratio of 2:1 and a rotation speed of 200r/min for 10 hours. The obtained slurry is filtered through a 100-mesh sieve after rotary evaporation, and the powder is molded under the pressure of 100 MPa. And (4) preserving the temperature of the demoulded blank in an oven for 2h at 120 ℃. And (4) placing the dried blank body in a high-temperature sintering furnace, and preserving the heat for 5 hours at 1100 ℃. The porosity of the prepared hydroxyapatite porous ceramic is 26.7%, and the compressive strength is 12.7 MPa.
Example 3:
100g of hydroxyapatite ceramic powder with the average particle size of 1.0 mu m, 200g of deionized water, 0.6g of polyacrylamide, 2.0g of polyethylene glycol and 15g of polymethyl methacrylate microspheres are weighed, zirconia balls are used as ball milling media, the ball-material ratio is 4:1, and the materials are mixed for 12 hours at the rotating speed of 100 r/min. The obtained slurry is filtered by a 200-mesh sieve after rotary evaporation, and the powder is molded by mechanical pressing under the pressure of 150 MPa. Keeping the demoulded blank in an oven at 150 ℃ for 0.5 h; and placing the dried blank body in a high-temperature sintering furnace, and preserving the heat for 3 hours at 1250 ℃. The porosity of the prepared hydroxyapatite porous ceramic is 18.5%, and the compressive strength is 18.9 MPa.
Example 4:
100g of hydroxyapatite ceramic powder with the average particle size of 0.5 mu m, 200g of deionized water, 0.8g of polyacrylamide, 1.0g of polyvinyl alcohol, 15g of activated carbon powder and 15g of polymethyl methacrylate microspheres are weighed, zirconia balls are used as ball milling media, the ball-to-material ratio is 2:1, and the materials are mixed for 8 hours at the rotating speed of 400 r/min. The obtained slurry is filtered through a 100-mesh sieve after rotary evaporation, and the powder is molded under the pressure of 100 MPa. And (4) preserving the temperature of the demoulded blank in an oven for 4 hours at 100 ℃. And (4) placing the dried blank body in a high-temperature sintering furnace, and keeping the temperature of 1200 ℃ for 2 h. The porosity of the prepared hydroxyapatite porous ceramic is 36.1%, and the compressive strength is 12.4 MPa.
Example 5:
weighing 100g of hydroxyapatite ceramic powder with the average particle size of 2.0 mu m, 100g of deionized water, 0.5g of polyacrylamide, 4.0g of polyethylene glycol and 10g of polymethyl methacrylate microspheres, taking zirconia balls as ball milling media, mixing the materials at a ball-to-material ratio of 3:1 and a rotating speed of 500r/min for 6 hours. The obtained slurry is filtered by a 325-mesh sieve after rotary evaporation, and the powder is molded by mechanical pressing under the pressure of 200 MPa. And (4) preserving the demoulded blank in an oven for 3 hours at the temperature of 120 ℃. And (4) placing the dried blank body in a high-temperature sintering furnace, and preserving the heat for 2 hours at 1300 ℃. The porosity of the prepared hydroxyapatite porous ceramic is 14.7%, and the compressive strength is 22.1 MPa.
Claims (7)
1. A preparation method of hydroxyapatite porous ceramics used as artificial bones is characterized in that: the method comprises the steps of mixing materials, preparing a green body and sintering the green body; the specific process steps are as follows:
1) mixing materials: taking deionized water, a dispersing agent, a binder, hydroxyapatite ceramic powder and a pore-forming agent as initial raw materials, and carrying out ball milling and mixing to obtain slurry with stable dispersion; drying the obtained slurry in a rotary evaporator, and sieving for later use; the adding amount of the deionized water is 1-3 times of the mass of the hydroxyapatite ceramic powder; the addition amount of the dispersing agent is 0.5-1.0% of the mass of the hydroxyapatite ceramic powder; the addition amount of the binder is 1.0-4.0% of the mass of the ceramic powder; the hydroxyapatite ceramic powder has the purity of more than 99.5 percent and the average particle size of 0.1-2.0 mu m; the addition amount of the pore-forming agent is 10-40% of the mass of the hydroxyapatite ceramic powder;
2) preparing a blank body: performing mechanical pressing on the sieved powder, demolding, and drying in an oven;
3) sintering of the green body: and sintering the dried blank in an air atmosphere furnace to obtain the hydroxyapatite porous ceramic.
2. The method for preparing a hydroxyapatite porous ceramic usable as an artificial bone according to claim 1, wherein: the dispersant is one of ammonium polyacrylate and polyacrylamide.
3. The method for preparing a hydroxyapatite porous ceramic usable as an artificial bone according to claim 1, wherein: the binder is one of polyvinyl alcohol and polyethylene glycol.
4. The method for preparing a hydroxyapatite porous ceramic usable as an artificial bone according to claim 1, wherein: the pore-forming agent is one or a mixture of more of starch, activated carbon powder and polymethyl methacrylate microspheres.
5. The preparation method of the hydroxyapatite porous ceramic used as the artificial bone according to claim 1, wherein ball milling and mixing are performed, zirconia balls are used as a ball milling medium, and the ball-to-material ratio is 2: 1-4: 1; the ball milling speed is 100-500 r/min, and the ball milling time is 6-12 h; the screening mesh number is 60-325 meshes.
6. The method for preparing hydroxyapatite porous ceramic used as artificial bone according to claim 1, characterized in that the pressure of the mechanical compression molding is 30 to 200 MPa; the temperature in the drying process is 100-150 ℃, and the heat preservation time is 0.5-5 h.
7. The method for preparing hydroxyapatite porous ceramic used as artificial bone according to claim 1, wherein the sintering process is heat preservation at 1000-1300 ℃ for 2-5 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113372132A (en) * | 2021-06-15 | 2021-09-10 | 昆明理工大学 | Chlorapatite porous material and preparation method thereof |
| CN115572177A (en) * | 2021-07-05 | 2023-01-06 | 陈月端 | Bone filler prepared from natural calcium-containing waste and preparation method thereof |
| CN116477966A (en) * | 2023-04-26 | 2023-07-25 | 深圳市博迪科技开发有限公司 | Preparation method of hydroxyapatite-based porous ceramic without powder falling |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113372132A (en) * | 2021-06-15 | 2021-09-10 | 昆明理工大学 | Chlorapatite porous material and preparation method thereof |
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| CN115572177A (en) * | 2021-07-05 | 2023-01-06 | 陈月端 | Bone filler prepared from natural calcium-containing waste and preparation method thereof |
| CN116477966A (en) * | 2023-04-26 | 2023-07-25 | 深圳市博迪科技开发有限公司 | Preparation method of hydroxyapatite-based porous ceramic without powder falling |
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