CN111592362A - SI3N4Reinforced hydroxyapatite composite nano ceramic material and preparation method thereof - Google Patents
SI3N4Reinforced hydroxyapatite composite nano ceramic material and preparation method thereof Download PDFInfo
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Abstract
The present application relates to a SI3N4A reinforced hydroxyapatite composite nano ceramic material and a preparation method thereof. The invention firstly utilizes the solution jet spinning technology to prepare the material with porosity and specific surfaceSI with improved combination of product, bioactivity and mechanical strength3N4The reinforced hydroxyapatite composite nano ceramic material has high bending strength, strong fracture toughness and high compressive strength. Compared with the prior art, the bending strength and the fracture toughness are greatly improved, the bending strength of the composite ceramic material is 330-560 MPa, and the fracture toughness is 3.5-5.7 MPam1/2. The material has excellent biocompatibility and mechanical property, can be used as a bone replacement material with strong bearing capacity to meet the requirements of orthopedics clinic on the biological property and the mechanical property of the bone material, is used for bone tissue engineering or used as an organism bone replacement material or a biological support material, has various functions, is convenient for mass production, and has good application prospect.
Description
Technical Field
The application belongs to the field of bionic material preparationRelates to the preparation of a biological ceramic material, in particular to SI prepared by adopting a solution jet spinning technology3N4The hydroxyapatite composite ceramic is enhanced.
Background
The bioceramic material is required to have higher biological elasticity, biocompatibility and stable chemical characteristics, and can be made into various tissues and organs such as teeth, body bones and the like by utilizing the characteristics for repairing or replacing human bodies, and the bioceramic material has the advantages of good biocompatibility, corrosion resistance and the like as an inorganic biomedical material and is more and more valued by people.
The biological ceramics comprise inert biological ceramics, active biological ceramics and absorbable biological ceramics according to different activities in organisms, wherein hydroxyapatite is a representative of the active biological ceramic materials, the ceramic materials are concerned by scholars at home and abroad in preparation process, biocompatibility, drug carriers and other aspects, the hydroxyapatite is one of quaternary inorganic compound apatite and belongs to a hexagonal crystal system, and compared with other biological materials, the hydroxyapatite contains substances which are the same as inorganic substances of human hard tissues, so the hydroxyapatite has good biocompatibility and no biological toxicity with biological tissues, has bone inductivity, can provide a bracket and a channel for the growth of new bone tissues, and the aperture, the porosity and the communication inside the pores are decisive factors of the bone growth mode and quantity, but the mechanical property of the hydroxyapatite material in a wet physiological environment is poor, the material is brittle, and the research on the hydroxyapatite material aims to overcome the brittleness and fatigue damage of the hydroxyapatite biological ceramic material in a physiological environment and enable the hydroxyapatite biological ceramic material to be used as a bone replacement material with strong bearing capacity, so that the problem that how to improve the obdurability of the nano hydroxyapatite material and the biocompatibility so as to meet the requirements of orthopedics clinics on biological performance and mechanical performance is to be solved urgently is solved. SI (Standard interface)3N4Belongs to inert biological ceramics, is not easy to dissolve in human body, is combined with biological hard tissue into a mechanical lock, has high bending strength, strong fracture toughness and high compressive strength, and is an effective toughening and reinforcing material.
The solution jet spinning technology is a novel method for preparing micro-nano fibers, and compared with the traditional electrostatic spinning method, the method does not need an electric field environment, does not need high-voltage equipment or any conductive collector, is simpler in equipment, can be used for spinning at a higher injection speed, is easy to operate, is low in cost, and is higher in spinning efficiency. The selection range of raw materials is wider, the raw materials are not limited to polymers with higher dielectric constants, and the adopted solvent is easy to volatilize, free of toxicity and more environment-friendly. The solution jet spinning technique is to deposit the fibers on the surface of a substrate or carrier by dissolving the raw materials in a volatile solvent and treating the mixture solution with a pressurized gas flowing at a high speed to promote the volatilization of the solvent and the deposition refinement of the fibers. The prepared micro-nanofiber has wide commercial value, and can be applied to polymer reinforcement, medical treatment, PM2.5 filtration, electrical and optical devices and the like.
The invention firstly utilizes the solution jet spinning technology to prepare the SI with improved comprehensive properties in the aspects of porosity, specific surface area, bioactivity, mechanical strength and the like3N4Compared with electrostatic spinning, the production efficiency of the nano ceramic fiber prepared by adopting the solution jet spinning technology is improved by 5-8 times, the constraint of a high-voltage electric field is eliminated, the blocking phenomenon of high-concentration inorganic salt spinning mother liquor near the tip of a syringe needle is obviously reduced, the safety performance is high, and the spinning efficiency is high.
Disclosure of Invention
In order to solve the above problems, the following technical solutions have been proposed through intensive research.
SI prepared by adopting solution jet spinning technology under high-pressure airflow3N4The reinforced hydroxyapatite composite nano ceramic material is characterized in that: the composite ceramic material is (NH)4)2HPO4Solution, Ca (NO)3)2Mixing the solution, ammonia water solution and polyethylene glycol as raw materials, reacting, and adding SI3N4Mixing the nanometer powder and polyethylene glycol, magnetically stirring to obtain precursor solution, and passing the precursor solution throughThe solution spraying device is formed by pumping a gun mouth and simultaneously spraying high-pressure airflow into a collector, wherein (NH)4)2HPO4The concentration of the solution is 0.1-2.0 mol/L, Ca (NO)3)2The concentration of the solution is 0.05-1.0 mol/L, SI3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)220 to 60 percent of the total molar amount, the bending strength of the composite ceramic material is 330 to 560MPa, and the fracture toughness is 3.5 to 5.7MPam1/2。
Preferably, said (NH)4)2HPO4The concentration of the solution is 0.15-1.8 mol/L, Ca (NO)3)2The concentration of the solution is 0.1-1.0 mol/L.
Preferably, the bending strength of the composite ceramic material is 370-550 MPa, and the fracture toughness is 3.8-5.0 MPam1/2。
Preferably, SI3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)225 to 50 percent of the total molar amount.
SI3N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material comprises the following steps:
(1) respectively preparing (NH) with a solubility of 0.1-2.0 mol/L4)2HPO4The solution and Ca (NO) with the concentration of 0.05-1.0 mol/L3)2Mixing the two solutions, adding ammonia water to adjust the pH value of the reaction solution to 10-11, and adding SI after the reaction is finished3N4Magnetically stirring the nano powder and polyethylene glycol to obtain a uniform dispersion liquid, namely a precursor solution, (NH)4)2HPO4The solution is prepared by using a mixed solution of deionized water and absolute ethyl alcohol, and Ca (NO)3)2Preparing the solution by using absolute ethyl alcohol;
(2) metering the precursor solution prepared in the step (1) by a metering pump, pumping the precursor solution into a nozzle by a muzzle pump, spraying a thin flow from a spinneret orifice along with the precursor solution, and simultaneously blowing and stretching the thin flow by a high-pressure airflow spraying device to obtain the sedimentSI accumulated on the collector3N4A/hydroxyapatite composite material, wherein the airflow pressure is 50-80 psi;
(3) will SI3N4Sintering the/hydroxyapatite composite material at high temperature, and then cooling to obtain the SI3N4The reinforced hydroxyapatite composite nano ceramic material.
Preferably, said (NH)4)2HPO4The concentration of the solution is 0.15-1.8 mol/L, Ca (NO)3)2The concentration of the solution is 0.1-1.0 mol/L.
Preferably, the gas stream pressure in step (2) is 70 psi.
Preferably, the bending strength of the composite ceramic material is 370-550 MPa, and the fracture toughness is 3.8-5.0 MPam1/2。
Preferably, SI3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)225 to 50 percent of the total molar amount.
SI prepared by adopting solution jet spinning technology under high-pressure airflow3N4The reinforced hydroxyapatite composite nano ceramic material is applied as a biological bone tissue replacement material. A
Advantageous effects
The technical scheme provided by the invention has the beneficial effects that: the invention firstly utilizes the solution jet spinning technology to prepare the SI with improved comprehensive properties in the aspects of porosity, specific surface area, bioactivity, mechanical strength and the like3N4The reinforced hydroxyapatite composite nano ceramic material has high bending strength, strong fracture toughness and high compressive strength, and is an effective toughening and reinforcing material. Compared with the prior art, the bending strength and the fracture toughness are greatly improved, the bending strength of the composite ceramic material is 330-560 MPa, and the fracture toughness is 3.5-5.7 MPam1/2. The material has excellent biocompatibility and mechanical property, can be used as a bone replacement material with strong bearing capacity to meet the requirements of orthopedics clinic on the biological property and the mechanical property of the bone material, is used for bone tissue engineering or used as an organism bone replacement material or a biological scaffold material,the multifunctional electric heating cooker has various functions, is convenient for mass production, and has good application prospect. Compared with electrostatic spinning, the production efficiency of the nano ceramic fiber prepared by adopting the solution jet spinning technology is improved by 5-8 times, the constraint of a high-voltage electric field is eliminated, the phenomenon of blockage of the high-concentration inorganic salt spinning mother liquor near the tip of the syringe needle is obviously reduced, the safety performance is high, and the spinning efficiency is high.
Detailed Description
Example 1
SI3N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material comprises the following steps:
(1) respectively preparing (NH) with the solubility of 0.5mol/L4)2HPO4Solution and Ca (NO) concentration of 0.05mol/L3)2Mixing the two solutions, adding ammonia water to adjust pH of the reaction solution to 10.5, and adding SI after the reaction is finished3N4Magnetically stirring the nano powder and polyethylene glycol to obtain a uniform dispersion liquid, namely a precursor solution, (NH)4)2HPO4The solution is prepared by using a mixed solution of deionized water and absolute ethyl alcohol, and Ca (NO)3)2Preparing the solution by using absolute ethyl alcohol; SI (Standard interface)3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)225% of the total molar amount.
(2) Metering the precursor solution prepared in the step (1) by a metering pump, pumping the precursor solution into a spray head by a muzzle pump, spraying a thin flow from a spinneret orifice along with the precursor solution, and simultaneously carrying out high-speed airflow blowing and stretching on the thin flow by a high-pressure airflow spraying device to obtain SI deposited on a collector3N4A/hydroxyapatite composite wherein the gas flow pressure is 60 psi;
(3) will SI3N4Sintering the/hydroxyapatite composite material at high temperature, and then cooling to obtain the SI3N4The reinforced hydroxyapatite composite nano ceramic material has the bending strength of 357MPa and the fracture toughness of 3.81MPam1/2。
Example 2
SI3N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material comprises the following steps:
(1) respectively preparing (NH) with the solubility of 1.0mol/L4)2HPO4Solution and Ca (NO) concentration of 0.55mol/L3)2Mixing the two solutions, adding ammonia water to adjust pH of the reaction solution to 10.5, and adding SI after the reaction is finished3N4Magnetically stirring the nano powder and polyethylene glycol to obtain a uniform dispersion liquid, namely a precursor solution, (NH)4)2HPO4The solution is prepared by using a mixed solution of deionized water and absolute ethyl alcohol, and Ca (NO)3)2Preparing the solution by using absolute ethyl alcohol; SI (Standard interface)3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)245 percent of the total molar amount.
(2) Metering the precursor solution prepared in the step (1) by a metering pump, pumping the precursor solution into a spray head by a muzzle pump, spraying a thin flow from a spinneret orifice along with the precursor solution, and simultaneously carrying out high-speed airflow blowing and stretching on the thin flow by a high-pressure airflow spraying device to obtain SI deposited on a collector3N4A/hydroxyapatite composite wherein the gas flow pressure is 70 psi;
(3) will SI3N4Sintering the/hydroxyapatite composite material at high temperature, and then cooling to obtain the SI3N4The reinforced hydroxyapatite composite nano ceramic material has the bending strength of 393MPa and the fracture toughness of 4.2MPam1/2。
Example 3
SI3N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material comprises the following steps:
(1) respectively preparing (NH) with the solubility of 1.6mol/L4)2HPO4Solution and Ca (NO) concentration of 0.75mol/L3)2Mixing the two solutions, adding ammonia water to adjust pH of the reaction solution to 11, and adding SI after the reaction is finished3N4Nano powderAnd polyethylene glycol, magnetically stirring to obtain uniform dispersion, i.e. (NH) as precursor solution4)2HPO4The solution is prepared by using a mixed solution of deionized water and absolute ethyl alcohol, and Ca (NO)3)2Preparing the solution by using absolute ethyl alcohol; SI (Standard interface)3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)255% of the total molar amount.
(2) Metering the precursor solution prepared in the step (1) by a metering pump, pumping the precursor solution into a spray head by a muzzle pump, spraying a thin flow from a spinneret orifice along with the precursor solution, and simultaneously carrying out high-speed airflow blowing and stretching on the thin flow by a high-pressure airflow spraying device to obtain SI deposited on a collector3N4A/hydroxyapatite composite wherein the gas flow pressure is 70 psi;
(3) will SI3N4Sintering the/hydroxyapatite composite material at high temperature, and then cooling to obtain the SI3N4The reinforced hydroxyapatite composite nano ceramic material has the bending strength of 513MPa and the fracture toughness of 5.02MPam1/2。
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. SI prepared by adopting solution jet spinning technology under high-pressure airflow3N4The reinforced hydroxyapatite composite nano ceramic material is characterized in that: the composite ceramic material is (NH)4)2HPO4Solution, Ca (NO)3)2Mixing the solution, ammonia water solution and polyethylene glycol as raw materials, reacting, and adding SI3N4The nanometer powder and polyethylene glycol are magnetically stirred uniformly to obtain precursor solution, the precursor solution is pumped through a gun mouth of a solution spinning device and is sprayed into a collector by utilizing high-pressure airflow at the same time to form (NH)4)2HPO4The concentration of the solution is 0.1-2.0 mol/L, Ca (NO)3)2The concentration of the solution is 0.05-1.0 mol/L, SI3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)220 to 60 percent of the total molar amount, the bending strength of the composite ceramic material is 330 to 560MPa, and the fracture toughness is 3.5 to 5.7MPam1/2。
2. SI prepared by high-pressure jet solution spinning according to claim 13N4The reinforced hydroxyapatite composite nano ceramic material is characterized in that (NH)4)2HPO4The concentration of the solution is 0.15-1.8 mol/L, Ca (NO)3)2The concentration of the solution is 0.1-1.0 mol/L.
3. SI prepared by solution jet spinning according to claims 1-23N4The reinforced hydroxyapatite composite nano ceramic material is characterized in that the bending strength of the composite ceramic material is 370-550 MPa, and the fracture toughness is 3.8-5.0 MPam1/2。
4. SI prepared by solution jet spinning under high pressure air stream according to claims 1-33N4The reinforced hydroxyapatite composite nano ceramic material is characterized by comprising SI3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)225 to 50 percent of the total molar amount.
5. SI3N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material comprises the following steps:
(1) respectively preparing (NH) with a solubility of 0.1-2.0 mol/L4)2HPO4The solution and Ca (NO) with the concentration of 0.05-1.0 mol/L3)2Mixing the two solutions, and adding ammonia water to adjust the pH of the reaction solution to 10-11, adding SI after the reaction is finished3N4Magnetically stirring the nano powder and polyethylene glycol to obtain a uniform dispersion liquid, namely a precursor solution, (NH)4)2HPO4The solution is prepared by using a mixed solution of deionized water and absolute ethyl alcohol, and Ca (NO)3)2Preparing the solution by using absolute ethyl alcohol;
(2) metering the precursor solution prepared in the step (1) by a metering pump, pumping the precursor solution into a spray head by a muzzle pump, spraying a thin flow from a spinneret orifice along with the precursor solution, and simultaneously carrying out high-speed airflow blowing and stretching on the thin flow by a high-pressure airflow spraying device to obtain SI deposited on a collector3N4A/hydroxyapatite composite material, wherein the airflow pressure is 50-80 psi;
(3) will SI3N4Sintering the/hydroxyapatite composite material at high temperature, and then cooling to obtain the SI3N4The reinforced hydroxyapatite composite nano ceramic material.
6. An SI according to claim 53N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material is characterized in that (NH)4)2HPO4The concentration of the solution is 0.15-1.8 mol/L, Ca (NO)3)2The concentration of the solution is 0.1-1.0 mol/L.
7. An SI according to claim 53N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material is characterized in that the air flow pressure in the step (2) is 70 psi.
8. An SI according to claim 53N4The preparation method of the reinforced hydroxyapatite composite nano ceramic material is characterized in that the bending strength of the composite ceramic material is 370-550 MPa, and the fracture toughness is 3.8-5.0 MPam1/2。
9. An SI according to claim 53N4Enhanced phosphorus hydroxyThe preparation method of the limestone composite nano ceramic material is characterized in that SI3N4The addition amount of the nano powder is (NH)4)2HPO4And Ca (NO)3)225 to 50 percent of the total molar amount.
10. SI prepared by adopting solution jet spinning technology under high-pressure airflow3N4The reinforced hydroxyapatite composite nano ceramic material is applied as a biological bone tissue replacement material.
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| CN1699270A (en) * | 2005-05-17 | 2005-11-23 | 杭州市萧山区中医院 | Preparation method of hydroxyapatite/zirconium dioxide biological ceramic composite material and its products |
| CN105233346A (en) * | 2015-10-27 | 2016-01-13 | 深圳大学 | Porous biological support slurry, three-dimensional porous biological support and preparation method of support |
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