CN105754288A - Polyether-ether-ketone wear resistant composite material, preparation method and application thereof in mechanical polishing retaining rings - Google Patents
Polyether-ether-ketone wear resistant composite material, preparation method and application thereof in mechanical polishing retaining rings Download PDFInfo
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Abstract
Belonging to the technical field of polymer composite materials, the invention relates to a polyether-ether-ketone wear resistant composite material, a preparation method and application thereof in mechanical polishing retaining rings. The polyether-ether-ketone wear resistant composite material is composed of, by mass percentage, 90-99.99% of polyether-ether-ketone resin and the balance coupling agent modified graphene oxide, and is prepared by a melt blending process. In order to improve the dispersibility of graphene oxide, the coupling agent is employed to perform surface treatment on graphene oxide. The polyether-ether-ketone wear resistant composite material prepared by the method provided by the invention has the characteristics of good wear resistance, high strength, high temperature resistance and the like, the processing technology is simple, the processing cost is low, and the polyether-ether-ketone wear resistant composite material meets the material requirement of mechanical polishing retaining rings. The material greatly reduces the processing cost of mechanical polishing retaining rings, and prolongs the service life of mechanical polishing retaining rings.
Description
Technical field
The invention belongs to technical field of polymer composite materials, be specifically related to a kind of polyether-ether-ketone wearing composite material, preparation method and the application in machine glazed finish retaining ring thereof.
Background technology
Polyether-ether-ketone resin is the new special engineering plastics of a kind of aromatic series semi-crystalline state, has the extremely excellent combination properties such as high temperature resistant, resistance to chemical attack, high-modulus, high-fracture toughness, processability are good, and frictional behaviour and self-lubricating property are excellent.But as friction reducing abrasion resistant material, its anti-wear performance of pure polyether-ether-ketone resin is not ideal enough, it is therefore desirable to be modified filling to widen its application to it.
Graphene is mono-layer graphite carbon atomic layer, is two-dimensional structure material, and it shows good character in mechanics, optics, calorifics and electricity.In carbon-based material, Graphene, with the architectural characteristic of its uniqueness and the performance of excellence and production cost relative moderate, makes Graphene be applied at a lot of field of scientific studies.The Graphene of monolayer is reunited in a solvent, poor dispersion, and therefore the functionalization of Graphene and dispersibility are most important in the application.Chemical functional functionalized graphene is avoided that the single-layer graphene reunion in solvent phase, and major part retains Graphene essence.Containing substantial amounts of hydroxyl, carboxyl and epoxy isoreactivity functional group on graphene oxide, the existence of these oxygen-containing functional groups, utilize chemical reaction that graphene oxide is carried out surface modification so that it is and form effective interface cohesion between polymeric matrix, reach dispersed in the polymer.
Result of study about machine glazed finish retaining ring shows at present, and polyether-ether-ketone composite material is the ideal material preparing retaining ring at present, and it can meet the properties requirement of retaining ring, and can improve the wear-out life of retaining ring.
Summary of the invention
It is an object of the invention to provide a kind of polyether-ether-ketone wearing composite material, preparation method and apply in machine glazed finish retaining ring.
A kind of polyether-ether-ketone wearing composite material of the present invention, it is made up of polyether-ether-ketone resin and coupling agent modified graphene oxide, calculating by quality 100%, the weight/mass percentage composition of polyether-ether-ketone resin is 90～99.99%, and all the other are coupling agent modified graphene oxide.
Further, the melt index of described polyether-ether-ketone resin be 20～25g/10min (measured by XRZ-400 fusion index instrument, test condition: 400 DEG C, load dispel code weight 5kg, polymer loads test barrel preheating 5min), polyether-ether-ketone powder diameter 10～20um.
Further, described graphene oxide adopts the Hummers method improved to prepare, including pre-oxidation and two steps of oxidation,
Pre-oxidation: 2.0～3.0g potassium peroxydisulfate and 1.0～3.0g phosphorus pentoxide are joined in 10～15mL concentrated sulphuric acid (mass fraction is 96～98%), being stirred and heated to 75～95 DEG C makes it dissolve, and adds 2～5g graphite powder and continues stirring reaction 5～7h under 75～95 DEG C of conditions；It is down to room temperature after reacting completely, adds the dilution of 400～600mL deionized water, sucking filtration, with absolute ethanol washing, dry, obtain pre-oxidation graphite；
Oxidation: being joined by above-mentioned pre-oxidation graphite in the concentrated sulphuric acid (mass fraction is 96～98%) of 60～100mL ice bath, be slowly added to 6～10g potassium permanganate, temperature controls below 10 DEG C；It is warmed up to 30～40 DEG C of reaction 1～3h after addition, is slow added into 100～200mL deionized water, after continuing stirring 0.5～1h, add 500～700mL deionized water and 5～15mL hydrogen peroxide (mass fraction is 30%)；Finally by above-mentioned solution sucking filtration, with the salt acid elution of mass fraction 8～15%, again with absolute ethanol washing to neutral, dry, add the ultrasonic 0.5～1.5h of deionized water afterwards, it is made into the graphite oxide aqueous dispersions of 5～10mg/mL, dialyse 2～5 days, then by above-mentioned graphite oxide solution ultrasonic disperse 25～35min, sucking filtration, with absolute ethanol washing, obtain graphene oxide after drying.
A kind of preparation method of polyether-ether-ketone wearing composite material, its step is as follows:
A. coupling agent modified graphene oxide: take 0.1～0.8g graphene oxide and join in 10～100mL ethanol solution (mass fraction >=99.7%), ultrasonic agitation 20～40min, 0.5～3.5mL silane coupler (KH550 or DB551) is added drop-wise in above-mentioned solution, 5～15h is reacted under 65～85 DEG C of conditions, filter, wash post-drying, obtain coupling agent modified graphene oxide；
B. the coupling agent modified graphene oxide ultrasonic disperse obtained by step A is in ethanol solution, and concentration is 0.05～0.50g/10mL, and jitter time is 0.5～2h；
C. the coupling agent modified graphene oxide after the ultrasonic disperse obtained by step B and polyether-ether-ketone powder are scattered in dehydrated alcohol, ultrasonic disperse 10～30min, again at normal temperatures through the mechanical mixture of 20～30min, under 60～80 DEG C of conditions, after sucking filtration, dry 6～8h；
D. mixture dried for step C is joined in double screw extruder, extrusion mixing when 360～380 DEG C, pelletize, dry, then by dried pellet in injection machine melted, inject mould molding, obtain polyether-ether-ketone wearing composite material.
Polyether-ether-ketone wearing composite material prepared by the present invention can be applied in machine glazed finish retaining ring.In chemical mechanical polishing operation, in wafer periphery plus a retaining ring, the stress that so can alleviate crystal round fringes is concentrated, thus solving crystal column surface unbalance stress and causing " overground " phenomenon of crystal round fringes, makes the raw uniform polish surface with tight flatness tolerance of crystal column surface.Specifically polyether-ether-ketone wearing composite material being prepared into maintenance ring-like, as in figure 2 it is shown, retaining ring internal diameter is 301mm, external diameter is 345mm, and thickness is 7.05mm.
Compared with pure polyether-ether-ketone resin, the present invention adopts wearability is good, self lubricity is good coupling agent modified graphene oxide as filler, and it is carried out surface modification treatment to strengthen self and the polyether-ether-ketone matrix compatibility, improve the interface interaction power between packing material and matrix simultaneously.Compare pure polyether-ether-ketone by friction testing and have relatively low coefficient of friction and wear rate.Take full advantage of the self lubricity that graphene oxide self is good, and also illustrate that coupling agent modified graphene oxide and polyether-ether-ketone matrix have the good compatibility.Due to dispersibility and good interface compatibility in the base, in friction process, be conducive to stable, homogeneous transfer membrane to be formed, reduce the roughness in friction pair face, reduce coefficient of friction and wear rate.
The service life of machine glazed finish retaining ring, the wear rate low by uniform surface was determined, the polyether-ether-ketone wearing composite material of the present invention can meet the critical demands of retaining ring processing, including intensity, thermostability and polishing fluid composition compatibility.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscopic picture of the coupling agent modified graphene oxide adopting the Hummers method improved to prepare of the present invention；
As can be seen from the figure coupling agent modified surface of graphene oxide has a lot of fold pattern, illustrates that graphite flake layer is well opened in oxidizing process；
Fig. 2 is the machine glazed finish retaining ring structural representation of the polyether-ether-ketone composite material of the present invention.
In figure, light grey annulus is to be injected into annular by polyether-ether-ketone composite material by injection molding technology, and circular inside diameters is 300mm, and external diameter is 345mm, and thickness is 7.05mm.
Detailed description of the invention
Below by specific embodiment, technical scheme being illustrated, described embodiment is the specific descriptions of the claim to the present invention, and claim includes but not limited to described embodiment content.
Embodiment 1
First, adopting the hummers method improved to prepare graphene oxide, detailed process is as follows:
Pre-oxidation: 2.5g potassium peroxydisulfate and 2.5g phosphorus pentoxide are added in 12mL concentrated sulphuric acid (mass fraction is 98%), are stirred and heated to 80 DEG C and make it dissolve, adds 3g graphite powder and continues at 80 DEG C of stirring reaction 6h.Being down to room temperature after reacting completely, add 0.5L deionized water, sucking filtration, be washed till neutrality with dehydrated alcohol afterwards, at 65 DEG C, dry 8h, obtains pre-oxidation graphite.
Oxidation: being added to by above-mentioned pre-oxidation graphite in the concentrated sulphuric acid (mass fraction is 98%) of 80mL ice bath, be slowly added to 8g potassium permanganate, temperature controls at 5 DEG C.After adding, it is warmed up to 35 DEG C of reaction 3h, is slowly added to 150mL deionized water, after stirring 0.5h, adds 500mL deionized water and 10mL hydrogen peroxide (mass fraction is 30%).Above-mentioned solution is carried out sucking filtration, with the salt pickling of mass fraction 10%, afterwards with absolute ethanol washing to neutral, at 65 DEG C of dry 6h, add the ultrasonic 1h of deionized water afterwards, it is made into the graphite oxide aqueous dispersions of about 5mg/mL, dialyse 3 days, then ultrasonic disperse 30min, after sucking filtration, with absolute ethanol washing, obtain graphene oxide at 80 DEG C of dry 10h.
Surface modification treatment: take 0.10g graphene oxide and join in 15mL ethanol solution, ultrasonic agitation 30min, is added drop-wise in above-mentioned solution by 0.5mL Silane coupling agent KH550, reacts 10h at 75 DEG C, filter, wash post-drying, obtain coupling agent modified graphene oxide 0.12g.
By coupling agent modified graphene oxide 0.05g ultrasonic disperse in 10mL ethanol solution, concentration is 0.05g/10mL, and jitter time is 0.5h；
By the coupling agent modified graphene oxide after ultrasonic disperse and the polyether-ether-ketone (trade mark: 550UPF；Manufacturer: Changchun Jida special plastic engineering Co., Ltd；Melt index is 20～25g/10min, powder diameter 10～20um) powder 49.95g ultrasonic disperse is in 500mL ethanol solution, at normal temperatures through the mechanical mixture of 30min after dispersion 30min, in 80 DEG C of dry 8h after sucking filtration；
Above-mentioned dried mixture is joined in double screw extruder, extrusion mixing when 380 DEG C, pelletize, and pellet is dried, dried pellet is melted in injection machine, is injected separately into bending, stretches or friction mould molding, obtain polyether-ether-ketone composite material test bars.Tensile bars is dumbbell shape, is of a size of 4.0 × 9.0 × 40.0mm, and bending batten is of a size of 4.0 × 6.0 × 55.0mm, and friction batten is diameter 6.3mm, the cylindrical batten of height 18.8mm.
Embodiment 2
Graphene oxide preparation process and step in the present embodiment take the hummers method improved in embodiment 1 to prepare graphene oxide process；
Surface modification treatment: take 0.30g graphene oxide and join in 45mL ethanol solution, ultrasonic agitation 30min, is added drop-wise in above-mentioned solution by 1.5mL Silane coupling agent KH550, reacts 10h at 75 DEG C, filter, wash post-drying, obtain coupling agent modified graphene oxide 0.34g.
Being dispersed in 10mL anhydrous ethanol solvent by coupling agent modified graphene oxide 0.25g, concentration is 0.25g/10mL, ultrasonic disperse 0.5h；
By the coupling agent modified graphene oxide after ultrasonic disperse and the polyether-ether-ketone (trade mark: 550UPF；Manufacturer: Changchun Jida special plastic engineering Co., Ltd) powder 49.75g is scattered in 500mL alcoholic solution, at normal temperatures through the mechanical mixture of 20min after ultrasonic disperse 30min, in 80 DEG C of dry 8h after sucking filtration；
Above-mentioned dried mixture is joined in double screw extruder, extrusion mixing when 380 DEG C, pelletize, and pellet is dried, dried pellet is melted in injection machine, injects mould molding, obtain polyether-ether-ketone composite material test sample.
Embodiment 3
Graphene oxide preparation process and step in the present embodiment take the hummers method improved in embodiment 1 to prepare graphene oxide process.
Surface modification treatment: take 0.60g graphene oxide and join in 90mL ethanol solution, ultrasonic agitation 30min, is added drop-wise in above-mentioned solution by 3.0mL Silane coupling agent KH550, reacts 10h at 75 DEG C, filter, wash post-drying, obtain coupling agent modified graphene oxide 0.68g.
Taking coupling agent modified graphene oxide 0.50g and be dispersed in 10mL anhydrous ethanol solvent, concentration is 0.50/10mL, ultrasonic disperse 0.5h；
By the coupling agent modified graphene oxide after ultrasonic disperse and the polyether-ether-ketone (trade mark: 550UPF；Manufacturer: Changchun Jida special plastic engineering Co., Ltd) powder 49.50g is scattered in 500mL alcoholic solution, at normal temperatures through the mechanical mixture of 30min after ultrasonic disperse 30min, in 80 DEG C of dry 8h after sucking filtration；
Above-mentioned dried mixture is joined in double screw extruder, extrusion mixing when 380 DEG C, pelletize, and pellet is dried, dried pellet is melted in injection machine, injects mould molding, obtain polyether-ether-ketone composite material test sample.
Polyether-ether-ketone composite material embodiment 1,2,3 prepared according to following table test condition requirement, carries out material friction wear properties test after being processed into test bars by injection mould molding, and result is as follows:
The friction and wear behavior of embodiment 1～3 is above pure polyether-ether-ketone as can be seen from Table 1.The friction and wear behavior of embodiment 3 is best, is 1MPa in load, and the testing time is 2h, and test speed is under the DRY SLIDING of 200r/min, and coefficient of friction reduces 6.5% compared with pure material, and wear rate reduces 29%.
The hot strength of embodiment 1～3 and elongation at break all promote to some extent relative to pure polyether-ether-ketone as can be seen from Table 2, hot strength embodiment 1～3 improves 13.2%, 14.0%, 13.5% respectively, and elongation at break improves 23.4%, 41.0%, 4.8% respectively.Bending strength does not promote compared with pure polyether-ether-ketone.
Table 1: polyether-ether-ketone composite material polishing machine test result
Note: friction and wear behavior adopts UMT-2 (Bruker, Germany) test, according to ASTMG99-04 standard.
Table 2: polyether-ether-ketone composite material mechanical experimental results
Claims (5)
1. a polyether-ether-ketone wearing composite material, it is characterized in that: be made up of polyether-ether-ketone resin and coupling agent modified graphene oxide, calculating by quality and 100%, the weight/mass percentage composition of polyether-ether-ketone resin is 90～99.99%, and all the other are coupling agent modified graphene oxide；Coupling agent modified graphene oxide is to take 0.1～0.8g graphene oxide to join in 10～100mL ethanol solution, ultrasonic agitation 20～40min, then 0.5～3.5mL silane coupler is added drop-wise in above-mentioned solution, reacting 5～15h under 65～85 DEG C of conditions, filtration, washing post-drying prepare.
2. a kind of polyether-ether-ketone wearing composite material as claimed in claim 1, it is characterized in that: graphene oxide is to join in 10～15mL concentrated sulphuric acid by 2.0～3.0g potassium peroxydisulfate and 1.0～3.0g phosphorus pentoxide, being stirred and heated to 75～95 DEG C makes it dissolve, and adds 2～5g graphite powder and continues stirring reaction 5～7h under 75～95 DEG C of conditions；It is down to room temperature after reacting completely, adds the dilution of 400～600mL deionized water, sucking filtration, with absolute ethanol washing, dry, obtain pre-oxidation graphite；Being joined by pre-oxidation graphite in the concentrated sulphuric acid of 60～100mL ice bath again, be slowly added to 6～10g potassium permanganate, temperature controls below 10 DEG C；It is warmed up to 30～40 DEG C of reaction 1～3h after addition, is slow added into 100～200mL deionized water, after continuing stirring 0.5～1h, add 500～700mL deionized water and 5～15mL hydrogen peroxide；Finally by above-mentioned solution sucking filtration, with the salt acid elution of mass fraction 5～15%, again with absolute ethanol washing to neutral, dry, add the ultrasonic 0.5～1.5h of deionized water afterwards, it is made into the graphite oxide aqueous dispersions of 5～10mg/mL, dialyse 2～5 days, then by above-mentioned graphite oxide solution ultrasonic disperse 25～35min, sucking filtration, with absolute ethanol washing, obtain graphene oxide after drying.
3. a kind of polyether-ether-ketone wearing composite material as claimed in claim 1, it is characterised in that: silane coupler is KH550 or DB551.
4. the preparation method of the polyether-ether-ketone wearing composite material described in claim 1,2 or 3, its step is as follows:
1) by coupling agent modified graphene oxide ultrasonic disperse in ethanol solution, concentration is 0.05～0.50g/10mL, and jitter time is 0.5～2h；
2) by step 1) coupling agent modified graphene oxide after the ultrasonic disperse that obtains is scattered in dehydrated alcohol with polyether-ether-ketone powder, ultrasonic disperse 10～30min, again at normal temperatures through the mechanical mixture of 20～30min, under 60～80 DEG C of conditions, after sucking filtration, dry 6～8h；
3) by step 2) dried mixture joins in double screw extruder, mixing, the extrusion, pelletize, dry when 360～380 DEG C, then dried pellet is melted in injection machine, inject mould molding, obtain polyether-ether-ketone wearing composite material.
5. the application in machine glazed finish retaining ring of the polyether-ether-ketone wearing composite material described in claim 1,2 or 3.
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| CN106633626A (en) * | 2016-09-27 | 2017-05-10 | 广东银禧科技股份有限公司 | Graphene/polyetheretherketone composite powder material for SLS (Selective Laser Sintering) and preparation method |
| CN106633627A (en) * | 2017-01-05 | 2017-05-10 | 吉林大学 | Polyether-ether-ketone/nanometer zinc oxide/carbon fiber wear-resistant composite material and preparation method thereof, and application of composite material to mechanical polishing of retaining rings |
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| CN110922716B (en) * | 2019-12-11 | 2022-07-01 | 长沙理工大学 | Polyether-ether-ketone composite material and preparation method thereof |
| CN111184913A (en) * | 2020-01-13 | 2020-05-22 | 吉林大学 | Artificial bone composite material based on polyether-ether-ketone and preparation method thereof |
| CN111184913B (en) * | 2020-01-13 | 2021-06-04 | 吉林大学 | Artificial bone composite material based on polyether-ether-ketone and preparation method thereof |
| CN115091338A (en) * | 2022-06-29 | 2022-09-23 | 中国地质大学（北京） | Method for improving polishing efficiency of single crystal diamond by adding metal oxide nano particles |
| CN117887205A (en) * | 2023-11-29 | 2024-04-16 | 咖爷科技(苏州)有限公司 | Preparation method of wear-resistant self-lubricating resin material and application of wear-resistant self-lubricating resin material in vane pump |
| CN117887205B (en) * | 2023-11-29 | 2024-07-23 | 咖爷科技(苏州)有限公司 | Preparation method of wear-resistant self-lubricating resin material and application of wear-resistant self-lubricating resin material in vane pump |
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