CN113956609B - Wear-resistant antistatic polyether ether ketone based composite material and preparation method and application thereof - Google Patents

Abstract

The invention belongs to the technical field of polymer materials, and discloses an anti-wear and antistatic polyetheretherketone-based composite material and its preparation method and application. The preparation method comprises: mixing self-lubricating polyetheretherketone and carbon fibers uniformly through mechanical grinding, The mixed powder is obtained; then the mixed powder is placed under a vacuum condition with a pressure of 10-20 MPa for hot pressing and sintering treatment to obtain the anti-wear and antistatic polyetheretherketone-based composite material. The composite material of the invention has the characteristics of low friction coefficient, low wear rate, small friction static electricity, etc., and has simple preparation process and good controllability. The material is suitable for use at room temperature and 60°C to 260°C. As a solid lubricating material, it has important application prospects in the fields of aerospace and automobile manufacturing.

Description

An anti-wear and anti-static polyetheretherketone-based composite material and its preparation method and application

technical field

The invention relates to the technical field of polymer materials, in particular to an anti-wear and anti-static polyetheretherketone-based composite material and its preparation method and application.

Background technique

Polyether ether ketone is a kind of thermoplastic resin. As a special polymer material, polyether ether ketone has excellent heat resistance, friction resistance, corrosion resistance and good mechanical properties, which makes polyether ether ketone a An extremely attractive matrix material for composite materials widely used in the aerospace, medical device, automotive and electronics industries.

The polyether ether ketone-based composite materials in the prior art have different properties due to different preparation methods, and the currently mature polymer composite materials have good performance under room temperature, low speed and low load conditions. Excellent friction and wear performance, but the friction and wear performance decreases rapidly under the harsh conditions of high temperature, high speed and heavy load, which limits its application range.

Therefore, the present invention provides an anti-wear and anti-static polyetheretherketone-based composite material and its preparation method and application.

Contents of the invention

In order to solve the above-mentioned deficiencies in the prior art, the present invention provides an anti-wear and antistatic polyether ether ketone-based composite material and its preparation method and application. The composite material of the present invention can have good wear resistance in the range from room temperature to 260°C properties and good antistatic properties.

An anti-wear and anti-static polyetheretherketone-based composite material of the present invention and its preparation method and application are realized through the following technical solutions:

The first object of the present invention is to provide a method for preparing an anti-wear and antistatic polyetheretherketone-based composite material, comprising the following steps:

The self-lubricating polyether ether ketone and carbon fiber are uniformly mixed through mechanical grinding, and then placed under a vacuum condition with a pressure of 10-20 MPa for hot pressing and sintering treatment to obtain the anti-wear and antistatic polyether ether ketone-based composite material.

Further, the hot pressing sintering treatment is as follows: firstly, the temperature is raised from room temperature to 300°C at a heating rate of 50-60°C/min, and then the temperature is raised from 300°C to 350°C at a heating rate of 8-10°C/min, and kept warm 5~15min.

Further, the mass ratio of the self-lubricating polyetheretherketone to the carbon fiber is 4-19:1.

Further, the self-lubricating polyether ether ketone is PEEK 450G powder, and its particle size is 12.5 μm.

Further, the short carbon fiber has a density of 1.8 g/cm ³ , a cross-sectional diameter of 900 mesh, and an aspect ratio of 6-8:1.

Further, the density of the anti-wear and antistatic polyether ether ketone-based composite material is not more than 1.5 g/cm ³ .

Further, the mechanical grinding is a dry ball mill with a ball-to-material ratio of 1-2:1, a rotational speed of 200-300 r/min, and a ball-milling time of 4-8 hours.

Further, the grinding pot and the grinding balls of the ball mill are made of tungsten carbide cemented carbide.

Further, the self-lubricating polyether ether ketone is also subjected to drying treatment before ball milling, the drying temperature of the drying treatment is 90-110° C., and the drying time is 4-12 hours.

Further, the vacuum degree of the vacuum condition is 10 ⁻¹ to 10 ⁰ Pa.

The second object of the present invention is to provide an antiwear and antistatic polyether ether ketone based composite material prepared by the above preparation method.

The third object of the present invention is to provide an application of the anti-abrasion and antistatic polyether ether ketone-based composite material prepared by the above preparation method in anti-abrasion and antistatic materials.

Compared with the prior art, the present invention has the following beneficial effects:

In the present invention, the self-lubricating polyetheretherketone and short carbon fibers are firstly dried to remove moisture in the material, so that the carbon fiber powder can be better dispersed in the process of mixing with the polyetheretherketone matrix powder, thereby facilitating the hot-pressing sintering process In the process, the carbon fiber powder forms a connected conductive network, which reduces the static electricity generated by friction. In addition, in the sintering process of the present invention, the temperature is raised in two stages for sintering. First, the temperature is raised rapidly to 300°C, so that the mixed powder is fully heated in a short time to prepare for the reaction of the powder at high temperature, and then slowly heated to 350°C. While preventing the thermal insulation temperature from being unstable due to an excessively fast heating rate, it is also ensured that the powder in the cavity of the graphite mold is heated evenly, thereby forming a solid material with relatively high density.

The material of the invention has low density and high hardness; the friction coefficient is low and stable, the wear rate is low, and it has good lubricating performance; the frictional static electricity is low, and it has good antistatic performance; the preparation process of the invention is simple and easy to operate, and the formula And the adjustment of the process can control the properties of the material.

Description of drawings

Fig. 1 is the room temperature friction curve of the polyetheretherketone-based composite material prepared in Comparative Example 1 of the present invention at three temperatures;

Fig. 2 is the room temperature wear rate of polyetheretherketone-based composite materials prepared in Comparative Example 1 of the present invention at three temperatures;

Fig. 3 is the room temperature friction curve of the material of the present invention;

Fig. 4 is the room temperature wear rate of the material of the present invention; Wherein, the histogram is sequentially from left to right the material of comparative example 1, embodiment 1, embodiment 2, embodiment 3 and embodiment 4;

Fig. 5 is a tribostatic diagram of the material of the present invention; wherein, the histograms are the materials of Comparative Example 1, Example 1, Example 2, Example 3 and Example 4 from left to right.

Detailed ways

The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the drawings in the embodiments of the present invention.

Example 1

This embodiment provides an anti-wear and antistatic polyetheretherketone-based composite material. The anti-wear and antistatic polyetheretherketone-based composite material in this embodiment is prepared through the following steps:

According to the mass ratio of 95:5, the self-lubricating polyether ether ketone and the short carbon fiber were respectively weighed, and placed in a high-energy ball mill, and the ball-to-material ratio was 2:1, and mixed for 6 hours at a speed of 260r/min to obtain a mixed powder.

Put the obtained mixed powder into a graphite mold, and place it in a vacuum rapid hot-press sintering furnace with a pressure of 15MPa and a vacuum degree lower than 1× ^10-1 Pa for hot-press sintering, first at 55°C/min The heating rate was raised from room temperature to 300°C, and then from 300°C to 350°C at a rate of 9°C/min, and kept at a temperature of 10 minutes to obtain an anti-wear and antistatic polyetheretherketone-based composite material.

Example 2

This embodiment provides an anti-wear and antistatic polyetheretherketone-based composite material. The anti-wear and antistatic polyetheretherketone-based composite material in this embodiment is prepared through the following steps:

Weigh the self-lubricating polyether ether ketone and short carbon fibers respectively according to the mass ratio of 90:10, and place them in a high-energy ball mill, mix them for 6 hours at a speed of 260r/min at a ball-to-material ratio of 2:1, and obtain a mixed powder.

Put the obtained mixed powder into a graphite mold with the same size as that in Example 1, and place it in a vacuum rapid hot-pressing sintering furnace with a pressure of 15 MPa and a vacuum degree lower than 1×10 ^-1 Pa. Raise the temperature from room temperature to 300°C, then raise the temperature from 300°C to 350°C at a rate of 9°C/min, and keep it for 10 minutes to obtain an anti-wear and antistatic polyetheretherketone-based composite material.

Example 3

This embodiment provides an anti-wear and antistatic polyetheretherketone-based composite material. The anti-wear and antistatic polyetheretherketone-based composite material in this embodiment is prepared through the following steps:

According to the mass ratio of 85:15, the self-lubricating polyetheretherketone and short carbon fibers were weighed respectively, and placed in a high-energy ball mill, and mixed for 6 hours at a ball-to-material ratio of 260r/min at a speed of 260r/min to obtain a mixed powder.

Put the obtained mixed powder into a graphite mold with the same size as that in Example 1, and place it in a vacuum rapid hot-pressing sintering furnace with a pressure of 15 MPa and a vacuum degree lower than 1×10 ^-1 Pa. Raise the temperature from room temperature to 300°C, then raise the temperature from 300°C to 350°C at a rate of 9°C/min, and keep it for 10 minutes to obtain an anti-wear and antistatic polyetheretherketone-based composite material.

Example 4

This embodiment provides an anti-wear and antistatic polyetheretherketone-based composite material. The anti-wear and antistatic polyetheretherketone-based composite material in this embodiment is prepared through the following steps:

According to the mass ratio of 80:20, the self-lubricating polyetheretherketone and short carbon fibers were weighed respectively, and placed in a high-energy ball mill, and mixed for 6 hours at a speed of 260r/min at a ball-to-material ratio of 2:1 to obtain a mixed powder.

Put the obtained mixed powder into a graphite mold with the same size as that in Example 1, and place it in a vacuum rapid hot-pressing sintering furnace with a pressure of 15 MPa and a vacuum degree lower than 1×10 ^-1 Pa. Raise the temperature from room temperature to 300°C, then raise the temperature from 300°C to 350°C at a rate of 9°C/min, and keep it for 10 minutes to obtain an anti-wear and antistatic polyetheretherketone-based composite material.

Example 5

This embodiment provides an anti-wear and antistatic polyetheretherketone-based composite material. The anti-wear and antistatic polyetheretherketone-based composite material in this embodiment is prepared through the following steps:

According to the mass ratio of 95:5, the self-lubricating polyether ether ketone and short carbon fiber were weighed respectively, and placed in a high-energy ball mill, and mixed for 8 hours at a ball-to-material ratio of 1:1 at a speed of 200r/min to obtain a mixed powder.

Put the obtained mixed powder into a graphite mold, and raise the temperature from room temperature to 300°C at a rate of 50°C/min in a vacuum rapid hot-pressing sintering furnace with a pressure of 10 MPa and a vacuum degree lower than 1×10 ^-1 Pa , and then the temperature was raised from 300°C to 350°C at a rate of 8°C/min, and kept at a temperature of 30 minutes to obtain an anti-wear and antistatic polyetheretherketone-based composite material.

Example 6

This embodiment provides an anti-wear and antistatic polyetheretherketone-based composite material. The anti-wear and antistatic polyetheretherketone-based composite material in this embodiment is prepared through the following steps:

According to the mass ratio of 95:5, the self-lubricating polyether ether ketone and short carbon fiber were weighed respectively, and placed in a high-energy ball mill, and mixed for 4 hours at a speed of 300r/min at a ball-to-material ratio of 2:1 to obtain a mixed powder.

Put the obtained mixed powder into a graphite mold, place it in a vacuum rapid hot pressing sintering furnace with a pressure of 15 MPa and a vacuum degree lower than 1× ¹⁰⁰ Pa, and raise the temperature from room temperature at a heating rate of 60 °C/min to 300°C, then from 300°C to 350°C at a heating rate of 10°C/min, and kept at this temperature for 20 minutes to obtain an anti-wear and antistatic polyetheretherketone-based composite material.

Comparative example 1

The difference with embodiment 1 only lies in:

Without adding short carbon fibers, the polyether ether ketone powder was directly put into a drying oven for 12 hours to make it completely dry, and then it was put into a graphite mold with the same size as that in Example 1 for hot-press sintering. Other operations are the same as in Example 1.

Experimental part

In order to verify the performance of the anti-wear and antistatic polyetheretherketone-based composite material of the present invention, the following tests were carried out on the materials of Examples 1-4 and Comparative Example 1.

(1) The density and hardness of the material

The present invention uses the Archimedes principle to measure the density of the materials of Comparative Example 1 and Example 1; uses a digital display Shore hardness tester to test the hardness of the materials of Comparative Example 1 and Example 1, and the test results are shown in Table 1.

Table 1 Density and Shore hardness of materials

Test case Density (g/cm) Shore hardness (HD) Comparative example 1 1.3 85 Example 1 1.5 87

(2) Friction coefficient and wear rate of materials

The friction and wear performance of the present invention is evaluated by using a UMT-2 multifunctional friction and wear testing machine and a three-dimensional shape profiler.

According to the above test conditions, the present invention tests the friction coefficient and wear rate of the polyetheretherketone material in Comparative Example 1 at three molding temperatures (340°C, 345°C, 350°C), and obtains the friction curves of the three molding temperatures Figure (as shown in Figure 1) and wear rate graph (as shown in Figure 2), and according to Figure 1 and Figure 2 can obtain the material of comparative example 1 in three kinds of forming temperature respectively average coefficient of friction and wear rate, the result As shown in table 2.

It should be noted that the melting point of polyether ether ketone material is 343° C., so the present invention selects three preparation temperatures near the melting point for research. If the temperature is too low, the material does not melt, which is equivalent to pressing the material powder into shape, and the performance is poor; if the temperature is too high, the material is completely melted, and after the hot pressing process, the material flows out from the graphite mold and cannot be formed.

Table 2 The friction coefficient and wear rate of the material in Comparative Example 1 and the GCr15 steel ball pair

temperature(℃) T1(340) T2(345) T3(350) average coefficient of friction 0.34 0.27 0.26 Wear rate (10^-4mm³/Nm) 13.2 3.49 0.513

In order to verify the impact of different additions of short carbon fibers on the performance of the material, the present invention tested the coefficient of friction and the wear rate of the materials of Examples 1-4 and Comparative Example 1, and obtained the materials of Examples 1-4 and Comparative Example 1 respectively Friction curve diagram (as shown in Figure 3) and wear rate curve diagram (as shown in Figure 4), and according to Figure 3 and Figure 4 can obtain the material average friction coefficient and wear rate of embodiment 1-4 and comparative example 1 , and the results are shown in Table 3.

The friction coefficient and the wear rate of the material of table 3 embodiment 1-4 and comparative example 1 and the GCr15 steel ball matching pair

Test case Comparative example 1 Example 1 Example 2 Example 3 Example 4 average coefficient of friction 0.272 0.255 0.256 0.250 0.247 Wear rate (10^-5mm³/Nm) 18.5 2.59 1.35 0.88 0.56

(3) Antistatic performance test

The antistatic performance of the present invention was measured by using FMX-003 triboelectrostatic meter for the materials prepared in Examples 1-4 and Comparative Example 1. The test results are shown in Figure 5 and Table 4.

Among them, the test conditions of the FMX-003 friction electrometer are:

The dual ball is GCr15 steel ball, the load is 50N, the sliding line speed is 0.13m/s, the friction radius is 4mm, and the running time is 30min.

Table 4 embodiment 1-4 and comparative example 1 material and GCr15 steel ball matching pair of friction static electricity

Test case Comparative example 1 Example 1 Example 2 Example 3 Example 4 Average frictional static electricity (V) 213.33 193.33 166.67 43.33 3.33

According to the above Table 1-Table 4, it can be seen that the hardness of the material prepared by the present invention is improved compared with the comparative example, and the thermal conductivity is increased by 1.5 times. Due to the increase of hardness, the surface of the material has a certain supporting effect, thereby improving the friction and wear performance of the material; secondly, due to the increase of thermal conductivity, the heat of the friction surface is reduced, thereby reducing the wear of the material due to friction heat. The invention selects highly conductive carbon fibers to disperse into the matrix material, which not only plays a role of support and reinforcement, but also forms a connected conductive network in the matrix material, reducing frictional static electricity.

Apparently, the above-mentioned embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

Claims (7)

1. A preparation method of anti-wear and antistatic polyetheretherketone-based composite material, characterized in that, comprising the following steps: Self-lubricating polyether ether ketone and carbon fiber are uniformly mixed by mechanical grinding to obtain a mixed powder; then the mixed powder is placed under a vacuum condition with a pressure of 10-20 MPa for hot pressing and sintering to obtain the anti-wear and antistatic polyether ether Ketone-based composite materials; The hot pressing sintering treatment is as follows: first raise the temperature from room temperature to 300°C at a heating rate of 50-60°C/min, then raise the temperature from 300°C to 350°C at a heating rate of 8-10°C/min, and keep the temperature for 5-15min ; The mass ratio of described self-lubricating polyether ether ketone and carbon fiber is 4～19:1; The mechanical grinding is dry ball milling; The self-lubricating polyether ether ketone is also dried before ball milling, the drying temperature of the drying treatment is 90-110° C., and the drying time is 4-12 hours. 2. The preparation method according to claim 1, wherein the self-lubricating polyether ether ketone is PEEK 450 G powder, and its particle size is 12.5 μm; The carbon fiber has a density of 1.8 g/cm ³ , a cross-sectional diameter of 900 mesh, and an aspect ratio of 6-8:1. 3. The preparation method according to claim 1, characterized in that the density of the anti-wear and anti-static polyether ether ketone-based composite material is not more than 1.5 g/cm ³ . 4. The preparation method according to claim 1, characterized in that the ball-to-material ratio of the dry ball mill is 1-2:1, the rotating speed is 200-300 r/min, and the ball-milling time is 4-8 h. 5. The preparation method according to claim 1, characterized in that the vacuum degree of the vacuum condition is 10 ⁻¹ ~10 ⁰ Pa. 6. A wear-resistant and antistatic polyetheretherketone-based composite material prepared by the preparation method according to any one of claims 1-5. 7. An application of the anti-wear and antistatic polyetheretherketone-based composite material according to claim 6 in anti-wear and antistatic materials.

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