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Polyether-ether-ketone material and surface modification method thereof

A polyetheretherketone and modification technology, which is applied in the field of surface modification of medical polymer materials, can solve the problems of unfavorable clinical medicine, poor biological activity, difficult bone tissue bonding, etc., and achieves improvement of initial adhesion and spreading conditions, The effect of improved alkaline phosphatase activity and simple and easy operation method

Inactive Publication Date: 2014-06-18
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the biological activity of polyetheretherketone is poor, and it is not easy to bond with bone tissue after implantation in the human body, which limits its long-term use as an implant material.
[0003] At present, there are several general methods to improve the problem of poor biocompatibility of polyetheretherketone materials: one is to use bioactive materials for compounding (such as tricalcium phosphate and hydroxyapatite, etc.), although this method can Effectively improve the biocompatibility of polyether ether ketone, but greatly sacrifice its inherent good mechanical properties, which is not conducive to its clinical application
The other is to apply a bioactive coating (such as titanium oxide, hydroxyapatite, etc.) on the surface of the material. This method can basically maintain the original mechanical properties of the polyether ether ketone matrix, but there are matrix and coating The firmness of the combination between them also limits its clinical application
Another method is to graft active functional groups (such as amino groups and carboxyl groups) on the surface of polyether ether ketone through chemical reactions. Although this method can also achieve the expected modification effect, it often requires multiple reaction steps, resulting in cumbersome operations. , time-consuming disadvantages

Method used

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  • Polyether-ether-ketone material and surface modification method thereof
  • Polyether-ether-ketone material and surface modification method thereof
  • Polyether-ether-ketone material and surface modification method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] After the pure polyetheretherketone of 10mm×10mm×1mm is polished, it is ultrasonically cleaned with acetone and deionized water in sequence, each time for 30 minutes, after cleaning, it is dried in an oven at 80°C and stored properly. Using the mixed gas of argon and water vapor as the ion source, plasma immersion ion implantation is carried out on the polyetheretherketone substrate, and the implanted modified polyetheretherketone material (AW-PEEK) is properly preserved. For the specific process parameters, see Table 2 shows.

[0045] Table 2 Argon water vapor mixed gas plasma immersion ion implantation parameters

[0046] Background vacuum (Pa)

[0047] figure 1 (AW-PEEK) is the surface morphology diagram of the medical polyetheretherketone material obtained through the modification treatment of this example. The figure shows that the surface of the modified material has narrow and long groove-like nanostructures; figure 2 (AW-PEEK) is a three-dimensional...

Embodiment 2

[0049] X-ray photoelectron spectroscopy (XPS) was used to evaluate the chemical state of the surface of the polyether ether ketone material obtained through the modification treatment of the above Comparative Example 1 and Example 1. The specific method is as follows: use a magnesium target Kα system (1253.6eV) ray source to measure the C1s and O1s high-resolution spectrum on the surface of the sample, and calculate the area percentage of each fitting peak in the high-resolution spectrum, and compare it with the measured sample The surface atomic percentages are listed together in Table 3. In addition, in order to qualitatively characterize the existence of hydroxyl groups on the surface of the material, a chemical derivatization method was used to label the hydroxyl groups as fluorine elements. Specifically, in the medium of pyridine and benzene, trifluoroacetic anhydride (TFAA) reacted with the hydroxyl groups on the surface of the sample to be tested (Analytical Chemistry 1...

Embodiment 3

[0055] The initial evaluation of the cytocompatibility of the polyether ether ketone material obtained through the modification of the above Comparative Example 1 and Example 1 was performed using the attachment and spreading of MC3T3 osteoblasts in the initial stage of in vitro culture. Methods as below:

[0056] 1) Put the sample sterilized with 75% ethanol into a 24-well culture plate, add 1 mL to each well with a density of 2×10 5 cell / mLMC3T3 cell suspension;

[0057] 2) Put the cell culture plate into 5% CO 2 Incubate at 36.5°C for 60 minutes in a cell culture incubator with saturated humidity;

[0058] 3) Aspirate the cell culture medium, wash the surface of the sample with PBS, move the sample to a new 24-well plate, add 2.5% glutaraldehyde solution to the sample to fix the cells, and the fixation time is not less than 4 hours;

[0059] 4) Aspirate the glutaraldehyde solution, add 30%, 50%, 75%, 90%, 95%, and 100% ethanol in sequence to dry and dehydrate the cells, ...

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Abstract

The invention relates to a polyether-ether-ketone material and a surface modification method thereof. The method comprises the step of carrying out plasma immersion ion implantation on a polyether-ether-ketone material by taking argon and water vapor as ion sources, wherein the process parameters of the plasma immersion ion implantation technique are as follows: the implantation voltage is 500-1000V, the argon flow is 15-60 sccm, the radio-frequency power is 300-500W, the base pressure is 5*10<-3> Pa, the duty ratio is 30%, the frequency is 30 kHZ, the implantation time is 30-90 minutes, the vacuum chamber temperature is 80-120 DEG C, and after the water vapor is fed, the vacuum chamber pressure is greater than 5*10<-3> Pa and smaller than 1*10<-2> Pa. The surface of the modified polyether-ether-ketone material is of a gully-shaped nanostructure, and the surface of the modified polyether-ether-ketone material is connected with a hydroxyl functional group.

Description

technical field [0001] The invention relates to a polyether ether ketone material and a method for surface modification thereof, in particular to a polyether ether ketone material obtained by plasma immersion ion implantation technology and a method for surface modification thereof, belonging to the surface modification method of medical polymer materials Modification technology field. Background technique [0002] In recent years, with the continuous development and improvement of the theory and technology of biomaterial preparation and use, high-performance polymer implant materials are expected to gradually replace titanium and its alloy materials, and the application prospects will be broader. The elastic modulus of polyetheretherketone matches that of human bone tissue. After implantation in the human body, it can effectively reduce bone resorption and bone atrophy caused by the stress shielding effect, and the polyetheretherketone material is resistant to chemical corr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/28C08L71/08C08K7/06C08K3/04
Inventor 刘宣勇王贺莹
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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