Polyetheretherketone composite and method of preparing same

Abstract

The invention provides a polyetheretherketone (PEEK) composite and a method of preparing same. The PEEK composite is prepared from 55-90 parts by mass of PEEK, 5-30 parts by mass zinc aluminum (ZA) alloy, 5-15 parts by mass graphite, 0.3-1 parts by mass graphene oxide (GO) and a processing additive. The PEEK composite is prepared by the following steps: putting the ZA alloy into an aqueous solution of a quaternary ammonium salt surfactant, ultrasonically dispersing, filtering, washing and drying; dissolving the GO in deionized water, dispersing the ZA alloy in deionized water, and adding a GO solution dropwise to a ZA alloy dispersion to obtain a GO/ZA alloy complex; mixing the PEEK, the GO/ZA alloy complex, the graphite and the processing additive, and drying at 100-120° C. for 3-4 h; and mixing in a mixer, and carrying out compression molding at 380-400° C.

Claims

1. A polyetheretherketone (PEEK) composite, wherein the PEEK composite is prepared from about 55-90 parts by mass of PEEK, about 5-30 parts by mass of zinc aluminum (ZA) alloy, about 5-15 parts by mass of graphite, about 0.3-1 parts by mass of graphene oxide (GO) and a processing additive; the ZA alloy is prepared from the following raw materials: about 90.5-91.1 parts by mass of zinc, about 8.5-8.6 parts by mass of aluminum, about 1.1-1.2 parts by mass of copper, and trace amounts of iron and magnesium impurities; the ZA alloy is present in the PEEK composite as a flake-like alloy powder, and the flake-like alloy powder is made by making the raw materials into powder by a smelting-nitrogen atomization method, and then making the powder into the flake-like alloy powder by a wet ball milling method; a melting point of the ZA alloy is 360-400° C.; the PEEK composite is prepared by the following steps: putting the flake-like ZA alloy powder into an aqueous solution of a quaternary ammonium salt surfactant, ultrasonically dispersing for more than 30 min, filtering, washing with deionized water and drying; ultrasonically dispersing and dissolving the GO in deionized water to obtain a GO solution, ultrasonically dispersing the ZA alloy processed by the above step in deionized water to obtain a ZA alloy dispersion, and adding the GO solution dropwise to the ZA alloy dispersion under stirring to obtain a GO and ZA alloy composite solution, and after the GO and ZA alloy composite solution is stratified, filtering the GO and ZA alloy composite solution to obtain a filter residue, and drying the filter residue, to obtain a GO/ZA alloy complex; mixing the PEEK, the GO/ZA alloy complex, the graphite and the processing additive to obtain a mixture, and drying the mixture at 100-120° C. for 3-4 h to obtain a dried material; and mixing the dried materials in a mixer to obtain a mixed material, and carrying out compression molding on the mixed material at 380-400° C.

2. The PEEK composite according to claim 1, wherein the GO is prepared by oxidation-exfoliation of graphite by a Hummers method.

3. The PEEK composite according to claim 1, wherein the GO is ultrasonically dispersed for more than 3 h and dissolved to a concentration of 0.01 g/mL.

4. The PEEK composite according to claim 1, wherein the processing additive comprises at least one of a lubricant and an antioxidant; the lubricant comprises 0.2-0.3 parts by mass of silicone oil or/and 0.2-0.3 parts by mass of polytetrafluoroethylene (PTFE); the antioxidant comprises 0.1-0.2 parts by mass of pentaerythritol tetrakys 3-(3,5-ditert-butyl-4-hydroxyphenyl)propionate or/and 0.1-0.2 parts by mass of tris-(2.4-di-tert-butyl)-phosphite.

5. The PEEK composite according to claim 1, wherein the preparation of the PEEK composite further comprises the following steps: heating the ZA alloy powder washed by deionized water to 100-110° C., stirring and drying for 10-15 min until a water content of the ZA alloy is less than 0.3%, putting the ZA alloy into a high-speed mixer, adding an aluminate coupling agent that is 0.8 wt % to 1.2 wt % of the ZA alloy powder, and blending the ZA alloy and the aluminate coupling agent for 3-5 min.

6. The PEEK composite according to claim 1, wherein the PEEK, the GO/ZA alloy complex, the graphite and an appropriate amount of processing additive are dried at 120° C. for 3 h after being mixed.

7. A polyetheretherketone (PEEK) composite, wherein the PEEK composite comprises about 55-90 parts by mass of PEEK, about 5-30 parts by mass of a zinc aluminum (ZA) alloy, about 5-15 parts by mass of graphite, about 0.3-1 parts by mass of graphene oxide (GO) and a processing additive; wherein the ZA alloy comprises about 90.5-91.1 parts by mass of zinc, about 8.5-8.6 parts by mass of aluminum, about 1.1-1.2 parts by mass of copper, and trace amounts of iron and magnesium impurities.

8. The PEEK composite according to claim 1, wherein the ZA alloy is a powder made by a smelting-nitrogen atomization method, and then processed into a flake-like alloy powder made by a wet ball milling method.

9. The PEEK composite according to claim 1, wherein a melting point of the ZA alloy is 360-400° C.

Description

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT(S)

(1) In order to help understand the invention, the invention is further described below with reference to the examples. The examples are merely intended to illustrate the invention, rather than to constitute a limitation to the invention in any way.

Example 1

(2) 90.5 parts by mass of zinc, 8.6 parts by mass of aluminum, 1.1 parts by mass of copper, and iron and magnesium impurities included in each material were made into zinc aluminum (ZA) alloy powder by a smelting-nitrogen atomization method. Then, flake-like alloy powder was prepared by a wet ball milling method. The melting point of the ZA alloy was controlled at 360-400° C.

(3) 5 parts by mass of the prepared flake-like ZA alloy powder were added into 0.3 mol/L aqueous solution of cetyl dimethyl ammonium bromide. The ZA powder was ultrasonically dispersed for more than 30 min, filtered, washed with deionized water, heated to 100-110° C., stirred and dried for 10-15 min until the water content thereof was less than 0.3%. Then the ZA alloy powder was put into a high-speed mixer, where an aluminate coupling agent DL-411 that was 0.8 wt % of the ZA alloy powder was added, and the materials were blended for 3 min.

(4) 0.3 parts by mass of graphene oxide (GO) were ultrasonically dispersed for more than 3 h and dissolved in deionized water, where the concentration of the GO was 0.01 g/mL. The ZA alloy processed in the above step was ultrasonically dispersed in deionized water to obtain a ZA alloy dispersion with a concentration of 0.1 g/ml. A GO solution was added dropwise to the ZA alloy dispersion under stirring and was filtered and dried after the solution is stratified, to obtain a GO/ZA alloy complex. The GO was prepared by oxidation-exfoliation of graphite by a Hummers method.

(5) 55 parts by mass of polyetheretherketone (PEEK), the GO/ZA alloy complex obtained in the above step, 5 parts by mass of graphite and 0.1 parts by mass of polytetrafluoroethylene (PTFE) were mixed, and then dried at 120° C. for 3 h.

(6) The materials were mixed in a mixer, and were subjected to compression molding at 380-400° C.

Example 2

(7) 91.1 parts by mass of zinc, 8.5 parts by mass of aluminum, 1.2 parts by mass of copper, and iron and magnesium impurities included in each material were made into ZA alloy powder by a smelting-nitrogen atomization method. Then, flake-like alloy powder was prepared by a wet ball milling method. The melting point of the ZA alloy was controlled at 360-400° C.

(8) 30 parts by mass of the prepared flake-like ZA alloy powder were added into 0.7 mol/L aqueous solution of octadecyl trimethyl ammonium chloride. The ZA powder was ultrasonically dispersed for more than 30 min, filtered, washed with deionized water, heated to 100-110° C., stirred and dried for 10-15 min until a water content thereof is less than 0.3%. Then the ZA alloy was put into a high-speed mixer, where an aluminate coupling agent DL-411 that was 1.2 wt % of the ZA alloy powder was added, and the materials were blended for 5 min.

(9) 1 part by mass of GO was ultrasonically dispersed for more than 3 h and dissolved in deionized water, where the concentration of the GO was 0.01 g/mL. The ZA alloy processed in the above step was ultrasonically dispersed in deionized water to obtain a ZA alloy dispersion with a concentration of 0.1 g/ml. A GO solution was added dropwise to the ZA alloy dispersion under stirring and was filtered and dried after the solution stratified, to obtain a GO/ZA alloy complex. The GO was prepared by oxidation-exfoliation of graphite by a Hummers method.

(10) 90 parts by mass of PEEK, the GO/ZA alloy complex obtained in the above step, 15 parts by mass of graphite and 0.2 parts by mass of antioxidant 1010 were mixed, and then dried at 100° C. for 4 h.

(11) The materials were mixed in a mixer, and were subjected to compression molding at 380-400° C.

Example 3

(12) 91 parts by mass of zinc, 8.55 parts by mass of aluminum, 1.15 parts by mass of copper, and iron and magnesium impurities included in each material were made into ZA alloy powder by a smelting-nitrogen atomization method. Then, a flake-like alloy powder was prepared by a wet ball milling method. The melting point of the ZA alloy was controlled at 360-400° C.

(13) 20 parts by mass of the prepared flake-like ZA alloy powder were added into 0.5 mol/L aqueous solution of dodecyl dimethyl benzyl ammonium chloride. The ZA powder was ultrasonically dispersed for more than 30 min, filtered, washed with deionized water, heated to 100-110° C., stirred and dried for 10-15 min until a water content thereof is less than 0.3%. Then the ZA alloy was put into a high-speed mixer, where an aluminate coupling agent DL-411 that was 1 wt % of the ZA alloy powder was added, and the materials were blended for 4 min.

(14) 0.6 parts by mass of GO were ultrasonically dispersed for more than 3 h and dissolved in deionized water, where the concentration of the GO was 0.01 g/mL. The ZA alloy processed in the above step was ultrasonically dispersed in deionized water to obtain a ZA alloy dispersion with a concentration of 0.1 g/ml. A GO solution was added dropwise to the ZA alloy dispersion under stirring and was filtered and dried after the solution stratified, to obtain a GO/ZA alloy complex. The GO was prepared by oxidation-exfoliation of graphite by a Hummers method.

(15) 75 parts by mass of PEEK, the GO/ZA alloy complex obtained in the above step, 10 parts by mass of graphite, 0.3 parts by mass of silicon oil and 0.2 parts by mass of antioxidant 168 were mixed, and then dried at 110° C. for 3.5 h.

(16) The materials were mixed in a mixer, and were subjected to compression molding at 380-400° C.

(17) The thermal deformation temperature, friction coefficient, wear loss, thermal conductivity, tensile strength, and impact strength of the PEEK composites obtained in each example and the PEEK were tested. The test results are shown in the following table.

(18) TABLE-US-00001 PEEK composites Items PEEK of Examples Thermal deformation temperature (° C.) 145 160-169 Friction coefficient 0.41 0.12-0.18 Wear loss (mg) 12.8 5-8 Thermal conductivity W/(m .Math. K) 0.2014 0.2665-0.4387 Tensile strength (MPa) 90  72-145 Impact strength (KJ/m.sup.2) 9.8 10.1-19.5

(19) The test results show that the tribological properties, thermal conductivity and mechanical properties of the PEEK composite obtained in the examples are significantly better than those of pure PEEK.

(20) In the invention, the thermal deformation temperature was tested according to ASTMD648 Standard Test Method for Deflection Temperature of Plastics Under Flexural Load in the Edgewise Position; the friction coefficient was tested according to GB 10006-1988 Plastics—Film and Sheeting—Determination of the Coefficients of Friction; the wear loss was tested according to GB/T 12444.1-1990 Metallic Materials—Wear Tests—MM Mode Wear Test; the thermal conductivity was tested according to ASTM D5470 Standard Test Method for Thermal Transmission Properties of Thermally Conductive Electrical Insulation Materials; the tensile strength was tested according to GB/T1040-2008 Plastics—Determination of Tensile Properties; the impact strength was tested according to GB/T1043.1-2008 Plastics—Determination of Charpy Impact Properties.

(21) The invention is not limited to the above preferred embodiments. Various changes and improvements may also be made within the spirit defined by the claims and specification of the invention. Such changes and improvements can solve the same technical problems and achieve the expected technical effects and are thus within the scope of the invention. All the solutions that those of ordinary skill in the art could conceive based on the disclosure of the invention are within the spirit defined by the claims and within the scope of the invention.