Method for preparing medical three-dimensional gradient netlike carbon fiber/ hydroxyapatite (HA)/ medical stone composite material

A composite material and carbon fiber technology, which is applied in medical science, anodic oxidation, prosthesis, etc., can solve the problems of low strength and poor toughness, and achieve the effect of good density and strength, less defects, and improved bonding ability

Inactive Publication Date: 2012-08-22

LIAONING UNIVERSITY OF TECHNOLOGY

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AI-Extracted Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the above-mentioned existing problems, and provide a preparation method of a three-dimensional gradient mesh carbon fiber/HA/medicine stone medical composite material; thi...

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Method used

B, add 0.95g dispersion agent ammonium polycarboxylate in 36.6ml deionized water, drip 15mol/L ammoniacal liquor again, the pH value of adjustment solution is 10, then add nanometer HA and nanometer medical stone and stir, again Ball milled for 24 hours to prepare a composite ceramic slurry with good dispersion and stability;

B,...

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Abstract

The invention discloses a method for preparing a medical three-dimensional gradient netlike carbon fiber/ hydroxyapatite (HA)/ medical stone composite material. The method comprises the following steps of: weaving carbon fibers into a three-dimensional gradient netlike carbon fiber skeleton; performing surface modification treatment on the three-dimensional gradient netlike carbon fiber skeleton;and making nano HA and nano medical stone composite ceramic slurry, compounding the composite ceramic slurry and the three-dimensional gradient netlike carbon fiber skeleton by adopting a centrifugalforming machine, sintering, and thus obtaining the composite material. The method has the advantages that the three-dimensional gradient netlike carbon fiber reinforcing effect is good, much HA can be compounded in a high-porosity area, and the composite material has good surface bioactivity; a low-porosity area has high carbon fiber content, so that the mechanical property of the HA matrix is improved; size completeness, few defects and high density of a blank of the composite material can be ensured by adopting the centrifugal grouting forming machine; and the nano medical stone added into the HA matrix contains a large quantity of trace elements which are beneficial to human body, and is used as a reinforcing phase for improving the strength of the HA matrix.

Application Domain

AnodisationProsthesis

Technology Topic

Composite materialSurface modification +7

Image

Examples

Experimental program(4)

Example Embodiment

[0028] Example 1

[0029] 1. The carbon fiber is woven into a three-dimensional gradient mesh carbon fiber skeleton with a porosity of 70% at both ends and a porosity of 40% at the core;

[0030] 2. DC-pulse anodization and alkali treatment of three-dimensional gradient mesh carbon fiber skeleton; 4 HCO 3 0.08mol/L, NH 4 H 2 PO 4 0.005mol/L, Ca(NO 3 ) 2 The 0.01mol/L configuration 3L electrolyte is poured into the electrolytic cell, the woven three-dimensional gradient mesh framework is immersed in the electrolyte as the anode, the graphite sheet is immersed in the electrolyte as the cathode, and a constant current is applied to the anode and the cathode. The current density is 150mA/g, the pulse current density is 300mA/g, the main pulse width is 0.3s, the auxiliary pulse width is 0.1s, the pulse frequency is 1Hz, and the oxidation time is 1min. The sample after DC-pulse anodization is cleaned with deionized water, then soaked in 0.5mol/L NaOH solution at 80℃ for 2 h, then cleaned with deionized water and dried to obtain a modified three-dimensional Gradient mesh carbon fiber skeleton;

[0031] 3. Configure a composite ceramic slurry with a solid phase percentage of 58wt%:

[0032] a. Take 51.4g nano HA, 6.6g nano medical stone, 42ml deionized water for use;

[0033] b. Add 0.29 g of dispersant ammonium polycarboxylate to 42 ml of deionized water, add dropwise ammonia water with a concentration of 15 mol/L, adjust the pH of the solution to 9, then add 51.4 g of nano HA and 6.6 g of nano medical stone, and stir Evenly, prepare multiphase ceramic slurry after ball milling for 24 hours;

[0034] 4. Inject the multiphase ceramic slurry into the modified three-dimensional gradient mesh carbon fiber skeleton in the centrifuge, and centrifuge for 90 minutes at a speed of 2500r/min to combine the nano HA and the nano HA in the multiphase ceramic slurry. The nano-medicine particles are deposited in the holes of the carbon fiber skeleton and form a dense accumulation with them to obtain the composite material green body. After demolding the composite material, it is dried at room temperature for 24 hours, and then sintered at 1100°C for 2 hours in a vacuum atmosphere, with an average heating rate of 5-10°C/min; it is made into three-dimensional gradient mesh carbon fiber/HA/medical stone Medical composite materials.

Example Embodiment

[0035] Example 2

[0036] 1. The carbon fiber is woven into a three-dimensional gradient mesh porous framework with a porosity of 65% at one end and a porosity of 40% at the other end. The pores show a continuous gradient decrease from the high pore end to the low pore end;

[0037] 2. Carry out DC-pulsed anodizing to remove NH 4 HCO 3 0.08mol/L, NH 4 H 2 PO 4 0.005mol/L, Ca(NO 3 ) 2 The 0.01mol/L configuration 3L electrolyte is poured into the electrolytic cell, the woven three-dimensional gradient mesh framework is immersed in the electrolyte as the anode, the graphite sheet is immersed in the electrolyte as the cathode, and a constant current is applied to the anode and the cathode. The current density is 50mA/g, the pulse current density is 100mA/g, the main pulse width is 0.3s, the auxiliary pulse width is 0.1s, the pulse frequency is 1Hz, and the oxidation time is 3min. The sample after DC-pulse anodization is cleaned with deionized water, then soaked in 0.5mol/L NaOH solution at 80℃ for 2 h, then cleaned with deionized water and dried to obtain a modified three-dimensional Gradient mesh carbon fiber skeleton;

[0038] 3. Configure the multi-phase ceramic slurry with the solid phase percentage of 76wt%:

[0039] a. Take 67.6g nano HA, 8.7g nano medical stone, 23.7ml deionized water;

[0040] b. Add 2.29g of dispersant ammonium polycarboxylate to 23.7ml of deionized water, then add dropwise 15mol/L ammonia to adjust the pH of the solution to 11, then add 67.6g of nano HA and 8.7g of nano medical stone and stir Evenly, prepare a multiphase ceramic slurry after ball milling for 24 hours;

[0041] 4. Inject the multiphase ceramic slurry into the modified three-dimensional gradient mesh carbon fiber skeleton in the centrifuge, and centrifuge for 30 minutes at 4000r/min to combine the nano HA and the nano HA in the multiphase ceramic slurry. The medical stone particles are deposited in the carbon fiber framework and form a dense accumulation with the carbon fiber skeleton to obtain the composite material green body. After demolding the composite material, it is dried at room temperature for 24 hours, and then sintered at 1280°C for 2 hours under an argon atmosphere, with an average heating rate of 5-10°C/min; that is, a three-dimensional gradient mesh carbon fiber/HA/Wheat Fanshi medical composite material.

Example Embodiment

[0042] Example 3

[0043] 1. The carbon fiber is woven into a three-dimensional gradient mesh carbon fiber skeleton with a porosity of 65% at both ends and a porosity of 50% at the core;

[0044] 2. Carry out DC-pulsed anodizing to remove NH 4 HCO 3 0.08mol/L, NH 4 H 2 PO 4 0.005mol/L, Ca(NO 3 ) 2 The 0.01mol/L configuration 3L electrolyte is poured into the electrolytic cell, the woven three-dimensional gradient mesh framework is immersed in the electrolyte as the anode, the graphite sheet is immersed in the electrolyte as the cathode, and a constant current is applied to the anode and the cathode. The current density is 100mA/g, the pulse current density is 200mA/g, the main pulse width is 0.3s, the auxiliary pulse width is 0.1s, the pulse frequency is 1Hz, and the oxidation time is 2min. The sample after DC-pulse anodization is cleaned with deionized water, then soaked in 0.5mol/L NaOH solution at 80℃ for 2 h, then cleaned with deionized water and dried to obtain a modified three-dimensional Gradient mesh carbon fiber skeleton;

[0045] 3. Configure the multiphase ceramic slurry with a solid phase volume content of 63.4wt%:

[0046] a. Take 56.2g nano HA, 7.2g nano medical stone, and 36.6ml as deionized water;

[0047] b. Add 0.95g of dispersant ammonium polycarboxylate to 36.6ml of deionized water, then add 15mol/L ammonia water dropwise to adjust the pH of the solution to 10, then add nano HA and nano medical stone, stir well, and then ball mill for 24 hours. Prepare a multi-phase ceramic slurry with good dispersibility and stability;

[0048] 4. Inject the multiphase ceramic slurry into the modified three-dimensional gradient mesh carbon fiber skeleton in the centrifuge, and centrifuge at 3000r/min for 60min to combine the nano HA and the nano HA in the multiphase ceramic slurry. The nano-medicine particles are deposited in the carbon fiber framework and form a dense accumulation with the carbon fiber framework to obtain the composite material green body. After demolding the composite material, it is dried at room temperature for 24 hours, and then sintered in a vacuum atmosphere at 1200°C for 2 hours, with an average heating rate of 5-10°C/min; that is, gradient mesh carbon fiber, nano HA, nano wheat rice are made Stone medical composite material.

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PUM

Property	Measurement	Unit
Particle size	40.0	nm
Density	3.17	g/cm³
Particle size	60.0	nm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Promote blood circulation
Reduce defects

Method for preparing medical three-dimensional gradient netlike carbon fiber/ hydroxyapatite (HA)/ medical stone composite material

A composite material and carbon fiber technology, which is applied in medical science, anodic oxidation, prosthesis, etc., can solve the problems of low strength and poor toughness, and achieve the effect of good density and strength, less defects, and improved bonding ability

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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