CN110819065A - Conductive wear-resistant light polyether ether ketone based composite material and preparation method thereof - Google Patents

Conductive wear-resistant light polyether ether ketone based composite material and preparation method thereof Download PDF

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Publication number
CN110819065A
CN110819065A CN201911086368.3A CN201911086368A CN110819065A CN 110819065 A CN110819065 A CN 110819065A CN 201911086368 A CN201911086368 A CN 201911086368A CN 110819065 A CN110819065 A CN 110819065A
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composite material
based composite
temperature
powder
ether ketone
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宋桂珍
扶肖肖
程建明
郭晓君
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/085Copper
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/04Antistatic

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A conductive wear-resistant light polyether ether ketone based composite material and a preparation method thereof belong to the field of polymer based composite materials, and the composite material is prepared from 35-45 parts by mass of polyether ether ketone, 50-60 parts by mass of electrolytic copper powder and 5 parts by mass of short carbon fiber; the preparation method comprises sieving polyetheretherketone powder, and drying at 110 deg.C for 4 hr; mechanically mixing polyether ether ketone powder, electrolytic copper powder and carbon fiber for 8 hours; the mixed material is put into a die for pressing at least 30min under the pressure of 30MPa and is sintered at high temperature; cooling to obtain the finished product. The friction coefficient of the invention is 0.30925-0.35878, and the volume abrasion loss is 3.2964-6.4562 mm3Volume resistivity of 2.00X 10‑2~1.316×10‑1Omega, m, density of 2.260632-2.670095 g/cm3

Description

Conductive wear-resistant light polyether ether ketone based composite material and preparation method thereof
Technical Field
The invention belongs to the field of polymer-based composite materials, and particularly relates to a conductive wear-resistant light polyether ether ketone-based composite material and a preparation method thereof.
Background
With the development of composite material technology, a single material cannot meet the increasing requirements of people on the material performance, and the composite material can not only make up the defects of the single material but also improve or enhance other performances required by people through the compounding of the material on the basis of keeping the physical properties of the original single material. Therefore, the composite material draws more and more attention of scientists due to the excellent comprehensive performance, and the composite material is widely applied to the daily life of people. The method is a very efficient way to obtain the conductive wear-resistant light polyether ether ketone based composite material by filling filler modified polyether ether ketone with the properties required by people.
One of the special engineering plastics of polyether-ether-ketone (PEEK) has good hot water resistance, can be used in high-pressure hot water and steam at 200 ℃ for a long time, has excellent creep resistance and fatigue resistance and good impact resistance, and is the best one of the special plastics. The flame retardant has better flame retardance, and the results of an NBS fuming experiment in the United states show that the fuming amount of the flame retardant is the lowest in all plastics, the flame retardant has chemical resistance, is insoluble in any other organic solvent except concentrated sulfuric acid, and has excellent electrical insulation, excellent processing performance, excellent biocompatibility and frictional wear. Is widely applied to aerospace, automobile industry, biomedical artificial bones, medical instruments, electric/electronic components, sealing components and the like. But it is an insulator with a volume resistivity of up to 1016Omega · m, good electrical insulation can be maintained even under high temperature environment. Therefore, the conductive wear-resistant light polyether ether ketone-based composite material needs to be modified. Copper resistivity of 1.7X 10-8Omega. m, excellent conductivity among metals, has been widely used as a conductive material due to its excellent ductility, good machinability, corrosion resistance, low price, and the like. The carbon fiber belongs to inorganic polymer fiber, has the advantages of high specific strength and specific modulus, excellent corrosion resistance, lower density, excellent conductivity, large specific surface area and the like, and is widely applied to the research of shielding materials, conductive materials and wear-resistant materials.
Disclosure of Invention
The invention provides a conductive wear-resistant light polyether-ether-ketone-based composite material with excellent conductivity, wear resistance and low density.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the conductive wear-resistant light polyether ether ketone based composite material is composed of the following raw materials in parts by weight:
35-45 parts of polyether-ether-ketone;
50-60 parts of electrolytic copper powder;
1-5 parts of short carbon fiber;
0.1-0.2 part of coupling agent;
wherein the electrolytic copper powder is subjected to surface treatment by a titanate coupling agent.
Preferably, the particle size of the electrolytic copper powder is 48 μm.
Preferably, the short carbon fibers have a diameter of 7 μm and a length of 1 to 3 mm.
The invention also discloses a preparation method of the conductive wear-resistant light polyether ether ketone based composite material, which comprises the following steps:
(1) sieving the first polyether-ether-ketone powder, then putting the sieved first polyether-ether-ketone powder into a drying oven for drying at the temperature of 110 ℃ for 4 hours, and sealing and packaging.
(2) The electrolytic copper powder is easy to oxidize in the air, and the electrolytic copper powder packaged in vacuum is weighed according to a certain mass fraction and then is treated by titanate coupling agent in time. And then sealing and storing.
(3) And adding the treated polyether ether ketone powder, the electrolytic copper powder and the carbon fiber into a ball milling tank of a planetary ball mill according to a certain mass ratio, and mechanically mixing for 8 hours to ensure that all materials are uniformly mixed.
(4) And putting the mixed material into a die cavity of a cold pressing die, carrying out die pressing on a press under the condition of room temperature, pressurizing to 30MPa, then maintaining the pressure for at least 30min under the pressure of 30MPa, and demoulding to take out a sample.
(5) Placing the demoulded cold-pressed part into a sintering mould, and carrying out three-stage sintering in a high-temperature furnace, wherein the temperature of the first stage is raised for 60 minutes from room temperature to 200 ℃; the second stage is a slow heating stage, wherein the temperature is increased from 200 ℃ to 310 ℃ for 60 minutes; the third stage is a heat preservation stage, and the temperature is preserved for 2 hours at 310 ℃; then cooling to room temperature for 4 hours to obtain the finished product.
According to the invention, the conductive property of the composite material is increased by filling the copper electrolysis powder filler in the polyether-ether-ketone, the interface action between two different substances can be improved after the treatment of the coupling agent, and the affinity of the composite material is improved so as to greatly improve the comprehensive performance of the composite material. The carbon fiber is filled with short carbon fiber, and has large specific surface area, so that the carbon fiber has good affinity with polyether-ether-ketone, and the interface binding force of the composite material is improved. Meanwhile, the carbon fiber has low density, good conductivity and friction and wear performance. The filling of the carbon fibers increases the conductivity of the composite material, improves the frictional wear performance of the composite material, and simultaneously improves the comprehensive performance of the composite material.
The conductive wear-resistant light polyether ether ketone-based composite material is prepared by filling modification, the mass fraction of electrolytic copper powder is preferably 50% -60%, then the mass fraction of the finally added short carbon fiber is preferably determined to be 5%, and the content of the electrolytic copper powder is most preferably 55%.
The friction coefficient of the invention is 0.30925-0.35878, and the volume abrasion loss is 3.2964-6.4562 mm3Volume resistivity of 2.00X 10-2~1.316×10-1Omega, m, density of 2.260632-2.670095 g/cm3
Detailed Description
The technical solution of the present invention will be described in detail, clearly and completely in the following with reference to the embodiments of the present invention.
Example 1
The polyether ether ketone based composite material is filled with the modified electrolytic copper powder with the mass fraction of 60 percent and the carbon fiber with the mass fraction of 5 percent.
The preparation method of the conductive wear-resistant light polyether ether ketone based composite material comprises the following steps:
and sieving the polyether-ether-ketone powder by using a screen, then drying the powder in a drying oven at 110 ℃ for 4 hours, and weighing 60 parts of electrolytic copper powder to perform surface treatment by using a coupling agent.
Adding 60 parts of electrolytic copper powder treated by the coupling agent, 35 parts of polyether-ether-ketone powder and 5 parts of short carbon fiber into a ball milling tank of a ball mill, and fully mixing to uniformly disperse the component materials.
Putting the mixed material into a cold pressing die of a tablet press, performing die pressing and pressurizing to 30MPa on the tablet press at room temperature, maintaining the pressure for 30 minutes under the pressure of 30MPa, and demolding to take out a sample;
and (3) placing the demoulded cold-pressed sample piece into a sintering mould, and carrying out high-temperature sintering in a high-temperature furnace in three stages, wherein the temperature is raised from room temperature to 200 ℃ in the first stage for 60 minutes, the temperature is slowly raised from 200 ℃ to 310 ℃ in the second stage for 60 minutes, the temperature is maintained at 310 ℃ in the third stage, the temperature is maintained for 2 hours at 310 ℃, and finally the cold-pressed sample piece is cooled to room temperature along with the furnace for 4 hours. And obtaining the polyether-ether-ketone-based composite material.
The conductive wear-resistant light polyether ether ketone based composite material prepared by the embodiment has the following properties: the coefficient of friction was 0.30925, and the volume abrasion loss was 3.2964 mm3The volume resistivity was 2.00X 10-2M, density 2.670095g/cm3
Example 2
The polyether ether ketone based composite material is filled with 55 mass percent of modified electrolytic copper powder and 5 mass percent of carbon fiber.
The preparation method of the conductive wear-resistant light polyether ether ketone based composite material comprises the following steps:
and sieving the polyether-ether-ketone powder by using a screen, then putting the powder into a drying oven to dry for 4 hours at 110 ℃, and weighing 55 parts of electrolytic copper powder to perform surface treatment by using a coupling agent.
Adding 55 parts of electrolytic copper powder treated by the coupling agent, 40 parts of polyether-ether-ketone powder and 5 parts of short carbon fiber into a ball milling tank of a ball mill, and fully mixing to uniformly disperse the component materials.
The process for pressing the sample and the process for sintering the sample were the same as in example 1.
The conductive wear-resistant light polyether ether ketone based composite material prepared by the embodiment has the following properties: the coefficient of friction was 0.31592, and the volume abrasion loss was 4.1048 mm3The volume resistivity was 3.67X 10-2M, density 2.401582 g/cm3
Example 3
The polyether ether ketone based composite material is filled with the modified electrolytic copper powder with the mass fraction of 50 percent and the carbon fiber with the mass fraction of 5 percent.
The preparation method of the conductive wear-resistant light polyether ether ketone based composite material comprises the following steps:
and sieving the polyether-ether-ketone powder by using a screen, then putting the powder into a drying oven to dry for 4 hours at 110 ℃, and weighing 50 parts of electrolytic copper powder to perform surface treatment by using a coupling agent.
Adding 50 parts of electrolytic copper powder treated by the coupling agent, 45 parts of polyether-ether-ketone powder and 5 parts of short carbon fiber into a ball milling tank of a ball mill, and fully mixing to uniformly disperse the component materials.
The process for pressing the sample and the process for sintering the sample were the same as in example 1.
The conductive wear-resistant light polyether ether ketone based composite material prepared by the embodiment has the following properties: the coefficient of friction was 0.35878, and the volume abrasion loss was 6.4562 mm3The volume resistivity was 1.316X 10-1M, density 2.260632 g/cm3
Performance testing shows that:
the invention cuts and polishes the finished product according to a certain specification, and tests the friction coefficient, the volume abrasion loss, the volume resistivity, the density and the like of the finished product.
Remarking: the performance detection conditions of the embodiments of the invention are as follows: friction and wear conditions: the method adopts a rotary friction wear mode, dry friction is carried out at room temperature, the diameter of a mating part is a steel ball with the diameter of 5mm, the material is GCr15, the wear rotation speed is 500r/min, the wear radius is 4mm, the load is loaded by 30N, and the friction time is 60 minutes.
The method for treating the electrolytic copper powder by the coupling agent comprises the following steps: weighing the electrolytic copper powder and the coupling agent reagent according to the mass ratio of 100:1, dropwise adding the coupling agent into the electrolytic copper powder while stirring, and ensuring that the electrolytic copper powder is fully treated.
When the mass fraction of the polyether-ether-ketone-based composite material prepared by the invention is 35-40 parts, the mass fraction of the electrolytic copper powder is 55-60 parts and the mass fraction of the short carbon fiber is 5 parts, the prepared polyether-ether-ketone-based composite material has good frictional wear property, and the resistivity reaches 10-2Omega, m, shows good conductivity,meanwhile, the density of the polyether ether ketone-based composite material is less than that of the aluminum alloy (2.7 g/cm)3) The composite material is a good light material, and is a novel polymer-based composite material with excellent conductive, wear-resistant and light properties.
The above mentioned is the preferable measure of the invention, the conductive wear-resistant light-weight polyether ether ketone based composite material is prepared by filling the modified polyether ether ketone with the electrolytic copper powder and the short carbon fiber according to a certain mass fraction, the filling components and the filling proportion of the composite material are equivalent changes made by the content of the specification of the invention, and the composite material is regarded as being in the protection scope of the invention without departing from the invention or directly or indirectly applying to other related technical fields.

Claims (8)

1. The conductive wear-resistant light polyether ether ketone based composite material comprises the following components in parts by weight:
35-45 parts of polyether-ether-ketone powder;
50-60 parts of electrolytic copper powder;
1-5 parts of short carbon fiber;
0.1-0.2 part of coupling agent.
2. The electrically conductive, abrasion resistant, light weight polyether ether ketone based composite material according to claim 1, wherein said polyether ether ketone powder has a particle size of 300 mesh.
3. The electrically conductive, abrasion resistant, lightweight polyether ether ketone based composite material of claim 1, wherein the electrolytic copper powder particle size is 300 mesh.
4. The electrically conductive, abrasion resistant, light weight polyether ether ketone based composite material of claim 1, wherein the short carbon fibers have a length of 1-3 mm.
5. The electrically conductive, abrasion resistant, lightweight polyether ether ketone based composite material of claim 1, wherein the coupling agent is titanate coupling agent 201.
6. According to claim 1The friction coefficient of the conductive wear-resistant light polyether ether ketone-based composite material is 0.30925-0.35878, and the volume wear amount is 3.2964-6.4562 mm3Volume resistivity of 2.00X 10-2~1.316×10-1Omega, m, density of 2.260632-2.670095 g/cm3
7. The electrically conductive, wear resistant and lightweight polyether ether ketone based composite material according to any one of claims 1 to 6, characterized in that the preparation method comprises the following steps:
sieving the polyetheretherketone powder, then putting the polyetheretherketone powder into a drying oven for drying at the temperature of 110 ℃ for 4 hours, and then sealing and packaging for later use;
weighing the electrolytic copper powder packaged in vacuum, then timely treating the electrolytic copper powder by using a titanate coupling agent, and then sealing and storing;
adding the treated polyether-ether-ketone powder, the electrolytic copper powder and the short carbon fibers into a ball milling tank of a planetary ball mill, and mechanically mixing for 8 hours to ensure that all materials are uniformly mixed;
placing the mixed material into a cold-pressing die cavity, performing die pressing and pressurization on a tablet press to 30MPa at room temperature, maintaining the pressure at 30MPa for at least 30min, demolding and taking out a sample piece;
placing the demoulded cold-pressed sample piece into a sintering mould, and carrying out three-stage sintering in a high-temperature furnace, wherein the temperature of the first stage is raised for 60 minutes from room temperature to 200 ℃; the second stage is a slow heating stage, wherein the temperature is increased from 200 ℃ to 310 ℃ for 60 minutes; the third stage is a heat preservation stage, and the temperature is preserved for 2 hours at 310 ℃; then cooling to room temperature for 4 hours to obtain the finished product.
8. A preparation method of a conductive wear-resistant light polyether-ether-ketone-based composite material is characterized by comprising the following steps:
(1) sieving the polyetheretherketone powder by using a screen, then putting the polyetheretherketone powder into a drying oven to dry for 4 hours at 110 ℃, and weighing 55 parts of electrolytic copper powder to perform surface treatment by using a coupling agent;
(2) adding 55 parts of electrolytic copper powder treated by a coupling agent, 40 parts of polyether-ether-ketone powder and 5 parts of short carbon fiber into a ball milling tank of a ball mill, and fully mixing;
(3) putting the mixed material into a cold pressing die of a tablet press, pressurizing to 30MPa on the tablet press at room temperature, maintaining the pressure for 30 minutes under the pressure of 30MPa, and demoulding to take out a sample;
(4) putting the sample piece into a sintering mold, and carrying out high-temperature sintering in a high-temperature furnace in three stages, wherein the temperature of the first stage is raised to 200 ℃ from room temperature for 60 minutes, the temperature of the second stage is slowly raised to 310 ℃ from 200 ℃, the temperature of the third stage is maintained at 310 ℃ for 2 hours, and finally the temperature is cooled to room temperature along with the furnace temperature for 4 hours to obtain the product with the friction coefficient of 0.31592 and the volume abrasion amount of 4.1048 mm3The volume resistivity was 3.67X 10-2M, density 2.401582 g/cm3The polyether ether ketone based composite material.
CN201911086368.3A 2019-11-08 2019-11-08 Conductive wear-resistant light polyether ether ketone based composite material and preparation method thereof Pending CN110819065A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111205591A (en) * 2020-02-28 2020-05-29 大连疆宇新材料科技有限公司 Large-scale polyether-ether-ketone mould pressing blank capable of being cut by wire electrical discharge machining
CN113956609A (en) * 2021-11-25 2022-01-21 河南科技大学 Wear-resistant antistatic polyether ether ketone based composite material and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1847290A (en) * 2006-04-12 2006-10-18 福州大学 Whisker reinforced resin-base composite friction material and its prepn process
CN104927298A (en) * 2015-06-30 2015-09-23 吉林大学 Polyetheretherketone-base composite, preparing method thereof and application thereof in friction reduction and wear resistance
CN106243620A (en) * 2016-08-05 2016-12-21 大连路阳科技开发有限公司 A kind of polyether-ether-ketone heat-conductive composite material and its production and use

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1847290A (en) * 2006-04-12 2006-10-18 福州大学 Whisker reinforced resin-base composite friction material and its prepn process
CN104927298A (en) * 2015-06-30 2015-09-23 吉林大学 Polyetheretherketone-base composite, preparing method thereof and application thereof in friction reduction and wear resistance
CN106243620A (en) * 2016-08-05 2016-12-21 大连路阳科技开发有限公司 A kind of polyether-ether-ketone heat-conductive composite material and its production and use

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111205591A (en) * 2020-02-28 2020-05-29 大连疆宇新材料科技有限公司 Large-scale polyether-ether-ketone mould pressing blank capable of being cut by wire electrical discharge machining
CN113956609A (en) * 2021-11-25 2022-01-21 河南科技大学 Wear-resistant antistatic polyether ether ketone based composite material and preparation method and application thereof

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