CN109777036A - A kind of polyether-ether-ketone base wearing composite material and preparation method thereof - Google Patents
A kind of polyether-ether-ketone base wearing composite material and preparation method thereof Download PDFInfo
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Abstract
A kind of polyether-ether-ketone base wearing composite material and preparation method thereof, it is related to functional composite material production technical field, modified graphene nano micro-flake, polyether-ether-ketone, polytetrafluoroethylene (PTFE) are mixed and be placed in double screw extruder, through melting mixing and extruding pelletization, the wear-resisting compound particle of polyether-ether-ketone base is obtained.Polyether-ether-ketone base wearing composite material of the invention is the PTFE phase and nano-sheet graphene microchip evenly dispersed in the base by the way that " island " structure is presented in PEEK matrix, forms the fine and close nano combined transfer film surface being made of PEEK-PTFE- graphene in friction process to obtain excellent wearability；This " island " structure and morphology and nano combined microstructure make composite material have excellent mechanical property especially toughness simultaneously.
Description
Technical field
The invention belongs to functional composite material production technical fields.
Technical background
Polyether-ether-ketone (PEEK) be used as a kind of high performance semi-crystalline thermoplastic polymer, have excellent mechanical property,
Chemical inertness and extensive temperature use scope, good thermal stability, it is numerous in bearing material, bone implant, piston ring etc.
Field is widely used as the substitute of metal component.However, due to its great friction coefficient (under dry-charged plates, the coefficient of friction of PEEK
0.4) and stick-slip behavior it greater than, limits it and is widely applied.
In order to improve PEEK tribological property, many researchers are by adding various filler such as SiO2, Al2O3, carbon fiber
(CF), graphene, PTFE, carbon nanotube etc. and their various combinations.In these lubrication fillers, CF and PTFE particle
It is widely used due to its excellent performance.Carbon fiber not only has in terms of modulus and intensity than other fibers very big excellent
Gesture, and there is excellent self-lubricating property due to the graphite-structure on their surfaces.The friction of CF enhancing PEEK composite material
Performance study discovery is learned, addition CF can greatly improve wearability of PEEK under the conditions of different application, if seawater lubricates, water profit
Sliding and dry sliding wear.
PTFE is as a kind of important solid lubricant, because it is with good physical and chemical properties, such as low friction
Coefficient, good thermal stability and chemical stability are widely used to chemical process, Spacecraft guidance and control and biotechnology work
Industry.The study found that addition PTFE can dramatically the coefficient of friction for reducing PEEK composite material in dry sliding wear test.In addition,
Due to graphene, molybdenum disulfide (MoS2) etc. two dimensions (2D) material interlaminar bonding (Van der Waals force) is weaker, interlayer shear relatively holds
Easily etc. reasons and be widely studied.For example, due to the formation of transfer membrane and the beneficial lubricating action of graphene, in PEEK matrix
Graphene is added, coefficient of friction can be made to significantly reduce.
However, few people study the wear-resisting modified material of PTFE and PEEK matrix compatibility, and with nanometer two-dimensional material
Synergistic effect, the influence to PEEK composite material frictional behaviour and mechanical property.As the confirmation of numerous research institutes, on sliding circle
High-performance boundary film is formed on face to be of great significance to the boundary lubrication performance for improving friction system.Because of high performance boundary
Film can carry the important load generated by solid-solid contact.In addition, this boundary film can also be brought by separating friction
Direct friction enhance the wearabilities of polymer composites.Therefore, Nanostructure fabrication friction boundary film is to raising PEEK
Composite material frictional behaviour has far-reaching significance.
Summary of the invention
To solve the above problems, the purpose of the present invention is to provide a kind of new polyether-ether-ketone base is wear-resisting compound
Material.
Polyether-ether-ketone base wearing composite material of the present invention is by polyether-ether-ketone resin, polytetrafluoroethylene (PTFE) and modified graphene nanometer
Microplate forms, and in the 100 mass parts composite material, polyether-ether-ketone resin is 80~90 parts, polytetrafluoroethylene (PTFE) is 9.9~19.5
Part, modified graphene nano micro-flake are 0.1~0.5 part.
Compared with the wear-resisting modified composite material of conventional polyether ether ketone, the PTFE of " island " structure is presented in composite material of the present invention
" island " not only can be with toughening composition, moreover, " island " phase PTFE is easier to form interfacial film on sliding interface when friction；Simultaneously
By the loaded modified graphene nanosheet of spindle calcium carbonate can in PEEK matrix it is evenly dispersed；The present invention formed by
The ternary nano interfacial film that PEEK, PTFE and graphene are constituted, effectively improves the boundary lubrication performance of friction system.Just
It is since the characteristic of the intensity and heat-resisting, PTFE low-friction coefficient and the solid lubricity of graphene that form collection PEEK is
The nanometer transfer membrane of one, makes PEEK composite material exhibits go out excellent low-friction coefficient and low wear.Meanwhile PEEK is multiple
" island " structure is improved significantly compared to PEEK toughness in condensation material.In addition, composite material of the present invention has excellent add
Work performance is easy to injection molding and extrusion molding.
It is another object of the present invention to propose the preparation method of the above composite material.
Modified graphene nano micro-flake, polyether-ether-ketone, polytetrafluoroethylene (PTFE) are mixed and be placed in double screw extruder, through molten
Melt mixing and extruding pelletization, obtains the wear-resisting compound particle of polyether-ether-ketone base；The polyether-ether-ketone resin, polytetrafluoroethylene (PTFE) and modification
Zhan always feeds intake 80~90%, 9.9~19.5%, the 0.1~0.5% of quality to the quality that feeds intake of graphene nanosheet respectively.The present invention
Using melting extrusion prilling, it can reach and improve the mixed uniformly degree of compound.
Further, polytetrafluoroethylene (PTFE) of the present invention is extrusion grade polytetrafluoroethylene (PTFE), and polytetrafluoroethylene (PTFE) may be implemented in this
It is not decomposed under 380~390 DEG C of processing temperature.
In addition, the invention also provides the methods processed of modified graphene nano micro-flake, comprising the following steps:
1) graphene microchip, calcium hydroxide and water are mixed, obtains suspension；The wherein mixing of graphene microchip and calcium hydroxide
Mass ratio is 6.76: 1.
2) it is passed through carbon dioxide into suspension, carries out gas-solid reaction under conditions of reaction temperature is 60~70 DEG C；Institute
When stating the pH of gas-solid reaction reaction system finally and dropping to 7, stopping is passed through carbon dioxide gas, filters, and obtains calcium carbonate load stone
Black alkene filter cake is simultaneously dried, and i.e. modified graphene nano micro-flake is obtained.
The temperature of the gas-solid reaction is 60~70 DEG C.The reaction temperature can get the spindle carbonic acid of submicron-scale
Calcium, the graphene after making load are readily dispersed in polymeric matrix.
In-situ preparation inorganic submicron calcium carbonate is utilized in the method processed of the above modified graphene nano micro-flake, may be implemented
Efficiently isolation graphene microchip improves its dispersibility.
One area Qu Zhijiu heating temperature of double screw extruder of the present invention is respectively as follows: 375 DEG C of area's temperature, two area's temperature
380 DEG C of degree, three 380 DEG C of area's temperature, four 385 DEG C of area's temperature, five 385 DEG C of area's temperature, six 390 DEG C of area's temperature, seven area's temperature 385
DEG C, eight 385 DEG C of area's temperature, nine 380 DEG C of area's temperature；18~25rps of rate of feeding, 30~38rps of engine speed.Each area's temperature is set
Meter ensures that polymer is sufficiently plasticized, the setting of feeding and host speed is main consider the uniform of melting mixing effect and tie rod and
Continuity.
Detailed description of the invention
Fig. 1 is the variation comparison diagram of the coefficient of friction of composite material made from the embodiment of the present invention and comparative example at any time.
Fig. 2 is the rubbing surface power dissipation spectrogram of composite material made from the embodiment of the present invention.
Fig. 3 is the rubbing surface power dissipation spectrogram with composite material made from comparative example.
Specific embodiment
One, the preparation process of modified graphene nano micro-flake:
100 g graphene microchips, 14.8g calcium hydroxide are added in 1000.0 g water, stirring, after forming unit for uniform suspension, are led to
Enter carbon dioxide, gas-solid reaction is carried out under 60 DEG C of reaction conditions.
When being reacted to the pH value of suspension and being reduced to 7, stops ventilation, filtered, washing obtains calcium carbonate load graphene filter
Cake 120g, be placed in 80 DEG C of vacuum ovens drying 12 hours it is spare to get modified graphene nano micro-flake.
Two, the preparation process of composite material:
1, embodiment:
It scores by following parts by weight and also known as measures: 90 parts of polyether-ether-ketone, 9.9 parts of extrusion grade polytetrafluoroethylene (PTFE), modified graphene nanometer
0.5 part of microplate.
Above each raw material full dose is added to high-speed mixer and carries out mechanical mixture, then uniformly mixed material is added
Double screw extruder melting mixing and extruding pelletization.
After the pellet that melting mixing squeezes out is placed in 120 DEG C of baking oven 2h, through injection molding machine injection molding.Wherein, twin-screw squeezes
The parameter setting of machine out are as follows: 375 DEG C of area's temperature, two 380 DEG C of area's temperature, three 380 DEG C of area's temperature, four 385 DEG C of area's temperature, 5th area
385 DEG C of temperature, six 390 DEG C of area's temperature, seven 385 DEG C of area's temperature, eight 385 DEG C of area's temperature, nine 380 DEG C of area's temperature；Rate of feeding 18-
25rps, engine speed 30-38rps.
2, comparative example:
Score by following parts by weight and also known as measure: 90 parts of polyether-ether-ketone, 9.9 parts of ethylene-tetrafluoroethylene copolymer, modified graphene are received
0.5 part of microplate of rice.Wherein, ethylene-tetrafluoroethylene copolymer is extrusion grade ethylene-TFE copolymer (E.I.Du Pont Company
F46).
The above components full dose is first added to high-speed mixer and carries out mechanical mixture, then uniformly mixed material is added
Enter double screw extruder melting mixing and extruding pelletization.
After the pellet that melting mixing squeezes out is placed in 120 DEG C of baking oven 2h, through injection molding machine injection molding.Wherein twin-screw extrusion
The parameter setting of machine are as follows: 375 DEG C of area's temperature, two 380 DEG C of area's temperature, three 380 DEG C of area's temperature, four 385 DEG C of area's temperature, five Qu Wen
385 DEG C of degree, six 390 DEG C of area's temperature, seven 385 DEG C of area's temperature, eight 385 DEG C of area's temperature, nine 380 DEG C of area's temperature；Rate of feeding 18-
25rps, engine speed 30-38rps.
Three, product property is verified:
From figure 1 it appears that the coefficient of friction for the composite material that embodiment obtains is significantly lower than comparative example.With frictional experiment
Progress, experimental example obtain composite material in about 2000s antithesis steel loop can preliminarily form boundary film, then friction system
Several is gradually stable, illustrates that boundary film can continuously and stably exist in the composite material of embodiment acquirement；And comparative example obtains
Composite material in the trend that rises of coefficient of friction performance fluctuation, this is because boundary film is discontinuous and in friction process point
From effective antifriction function cannot be played.
Figure it is seen that PTFE is with " island " shape structure disperses in PEEK matrix in the composite material that embodiment obtains；
In addition fluorine element content is obviously increased compared to ontology known to power dissipation spectrogram result.This result explanation, embodiment obtain
Composite material in " island " shape structure PTFE be easier to be enriched in surface in friction process, with matrix PEEK and modified graphene
Fine and close ternary nano boundary film is collectively formed.The nanometer boundary film of proper proportion composition has low-friction coefficient and low wear
(table 1) is not easily disconnected under the conditions of strong mechanical friction, shows continuous-stable.
And ethylene-tetrafluoroethylene copolymer is evenly dispersed in PEEK matrix in the composite material that comparative example obtains, such as
Shown in Fig. 3, in addition do not occur the enrichment phenomenon of fluorine element in its power dissipation spectrogram result, the ternary nano boundary film of formation rubs
It is big to wipe coefficient, abrasion loss height (table 1).
Table 1: the mechanical property contrast table of composite material made from the embodiment of the present invention and comparative example.
| Project | Coefficient of friction | Abrasion loss/mg | Wear scar width/mm | Wear rate/(10-9cm3/Nm) |
| Embodiment | 0.266 | 1.9 | 2.90 | 1.01 |
| Comparative example | 0.323 | 3.2 | 3.58 | 3.28 |
As it can be seen from table 1 embodiment reveals excellent frictional behaviour compared to comparative example table.
Table 2: the frictional behaviour contrast table of composite material made from the embodiment of the present invention and comparative example.
| Project | Tensile strength/MPa | Elongation at break/% | Bending strength/MPa | Impact strength/KJ/m2 |
| Embodiment | 87.32 | 7.52 | 96.1 | 13.98 |
| Comparative example | 89.68 | 2.78 | 96.4 | 9.6 |
From table 2 it can be seen that embodiment is under conditions of intensity decline is few, toughness, which has, to be obviously improved, this is mainly
It, can effectively toughening PEEK since PTFE is dispersed in PEEK matrix with island structure.
Claims (5)
1. a kind of polyether-ether-ketone base wearing composite material, it is characterised in that the composite material is by polyether-ether-ketone resin, polytetrafluoro
Ethylene and modified graphene nano micro-flake composition, in the 100 mass parts composite material, polyether-ether-ketone resin is 80~90 parts,
Polytetrafluoroethylene (PTFE) is 9.9~19.5 parts, modified graphene nano micro-flake is 0.1~0.5 part.
2. the preparation method of polyether-ether-ketone base wearing composite material as described in claim 1, it is characterised in that by modified graphene
Nano micro-flake, polyether-ether-ketone, polytetrafluoroethylene (PTFE) mixing are placed in double screw extruder, through melting mixing and extruding pelletization, are taken
Obtain the wear-resisting compound particle of polyether-ether-ketone base；The throwing of the polyether-ether-ketone resin, polytetrafluoroethylene (PTFE) and modified graphene nano micro-flake
Zhan always feeds intake 80~90%, 9.9~19.5%, the 0.1~0.5% of quality to material quality respectively.
3. the preparation method of polyether-ether-ketone base wearing composite material according to claim 2, it is characterised in that the polytetrafluoro
Ethylene is extrusion grade polytetrafluoroethylene (PTFE).
4. the preparation method of polyether-ether-ketone base wearing composite material according to Claims 2 or 3, it is characterised in that the modification
The method processed of graphene nanosheet the following steps are included:
1) graphene microchip, calcium hydroxide and water are mixed, obtains suspension；The wherein mixing of graphene microchip and calcium hydroxide
Mass ratio is 6.76: 1；
2) it is passed through carbon dioxide into suspension, carries out gas-solid reaction under conditions of reaction temperature is 60~70 DEG C；The gas
Gu the pH for reacting reaction system finally drops to 7, stopping is passed through carbon dioxide gas, filters, and obtains calcium carbonate load graphene
Filter cake is simultaneously dried, and i.e. modified graphene nano micro-flake is obtained.
5. the preparation method of polyether-ether-ketone base wearing composite material according to claim 2, it is characterised in that the twin-screw
One area Qu Zhijiu heating temperature of extruder is respectively as follows: 375 DEG C of area's temperature, two 380 DEG C of area's temperature, three 380 DEG C of area's temperature, and four
385 DEG C of area's temperature, five 385 DEG C of area's temperature, six 390 DEG C of area's temperature, seven 385 DEG C of area's temperature, eight 385 DEG C of area's temperature, nine Qu Wendu
380℃；18~25rps of rate of feeding, 30~38rps of engine speed.
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Cited By (7)
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| CN110195266A (en) * | 2019-06-17 | 2019-09-03 | 扬州市维纳复合材料科技有限公司 | A kind of production method of functional fibre |
| CN110591283A (en) * | 2019-09-30 | 2019-12-20 | 新奥（内蒙古）石墨烯材料有限公司 | Conductive graphene composite material and preparation method and application thereof |
| CN113881173A (en) * | 2021-11-11 | 2022-01-04 | 中国科学院兰州化学物理研究所 | Self-lubricating fiber fabric composite material and preparation method and application thereof |
| CN113897024A (en) * | 2021-10-29 | 2022-01-07 | 东风商用车有限公司 | Wear-resistant polyether-ether-ketone material for protecting easily worn units and application thereof |
| CN114231165A (en) * | 2021-12-27 | 2022-03-25 | 扬州市维纳复合材料科技有限公司 | Polyphenylene sulfide powder coating and preparation method and application thereof |
| CN115073880A (en) * | 2022-07-22 | 2022-09-20 | 中国电子科技集团公司第三十八研究所 | Extrudable, toughened and modified polyether-ether-ketone material for aviation liquid cooling pipe system and preparation method thereof |
| CN116751381A (en) * | 2023-03-07 | 2023-09-15 | 江苏君华特种工程塑料制品有限公司 | Preparation method of high-performance carbon fiber reinforced PEEK prepreg and PEEK substrate material |
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| CN110195266A (en) * | 2019-06-17 | 2019-09-03 | 扬州市维纳复合材料科技有限公司 | A kind of production method of functional fibre |
| CN110195266B (en) * | 2019-06-17 | 2021-08-17 | 扬州市维纳复合材料科技有限公司 | Production method of functional fiber |
| CN110591283A (en) * | 2019-09-30 | 2019-12-20 | 新奥（内蒙古）石墨烯材料有限公司 | Conductive graphene composite material and preparation method and application thereof |
| CN110591283B (en) * | 2019-09-30 | 2023-01-17 | 内蒙古信敏惠纳米科技有限公司 | Conductive graphene composite material and preparation method and application thereof |
| CN113897024A (en) * | 2021-10-29 | 2022-01-07 | 东风商用车有限公司 | Wear-resistant polyether-ether-ketone material for protecting easily worn units and application thereof |
| CN113881173A (en) * | 2021-11-11 | 2022-01-04 | 中国科学院兰州化学物理研究所 | Self-lubricating fiber fabric composite material and preparation method and application thereof |
| CN113881173B (en) * | 2021-11-11 | 2022-06-03 | 中国科学院兰州化学物理研究所 | Self-lubricating fiber fabric composite material and preparation method and application thereof |
| CN114231165A (en) * | 2021-12-27 | 2022-03-25 | 扬州市维纳复合材料科技有限公司 | Polyphenylene sulfide powder coating and preparation method and application thereof |
| CN115073880A (en) * | 2022-07-22 | 2022-09-20 | 中国电子科技集团公司第三十八研究所 | Extrudable, toughened and modified polyether-ether-ketone material for aviation liquid cooling pipe system and preparation method thereof |
| CN116751381A (en) * | 2023-03-07 | 2023-09-15 | 江苏君华特种工程塑料制品有限公司 | Preparation method of high-performance carbon fiber reinforced PEEK prepreg and PEEK substrate material |
| CN116751381B (en) * | 2023-03-07 | 2023-12-08 | 江苏君华特种工程塑料制品有限公司 | Preparation method of high-performance carbon fiber reinforced PEEK prepreg and PEEK substrate material |
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