CN105754288B - Polyether-ether-ketone wearing composite material, preparation method and its application in terms of retaining ring is mechanically polished - Google Patents
Polyether-ether-ketone wearing composite material, preparation method and its application in terms of retaining ring is mechanically polished Download PDFInfo
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- CN105754288B CN105754288B CN201610125370.7A CN201610125370A CN105754288B CN 105754288 B CN105754288 B CN 105754288B CN 201610125370 A CN201610125370 A CN 201610125370A CN 105754288 B CN105754288 B CN 105754288B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
Abstract
A kind of polyether-ether-ketone wearing composite material, preparation method and its application in terms of retaining ring is mechanically polished, belong to technical field of polymer composite materials.It is made up of polyether-ether-ketone resin and coupling agent modified graphene oxide, is calculated by quality and 100%, the weight/mass percentage composition of polyether-ether-ketone resin is 90~99.99%, and remaining is coupling agent modified graphene oxide, is prepared by melt blending technique.In order to improve the dispersiveness of graphene oxide, graphene oxide is surface-treated with coupling agent.Polyether-ether-ketone wearing composite material prepared by the present invention has a preferable wearability, high intensity, and the features such as high temperature resistant, processing technology is simple, and processing cost is relatively low, and polyether-ether-ketone wearing composite material meets the material requirements of mechanical polishing retaining ring.This material greatly reduces the processing cost of mechanical polishing retaining ring, extends the service life of mechanical polishing retaining ring.
Description
Technical field
The invention belongs to technical field of polymer composite materials, and in particular to a kind of polyether-ether-ketone wearing composite material, system
Preparation Method and its application in terms of retaining ring is mechanically polished.
Background technology
Polyether-ether-ketone resin is a kind of new special engineering plastics of aromatic series semi-crystalline state, has high temperature resistant, chemically-resistant rotten
The extremely excellent combination properties such as erosion, high-modulus, high-fracture toughness, processability be good, and frictional behaviour and self-lubricating property are excellent
It is different.But friction reducing abrasion resistant material is used as, its anti-wear performance of pure polyether-ether-ketone resin is not ideal enough, it is therefore desirable to which it is modified
Fill to widen its application field.
Graphene is mono-layer graphite carbon atomic layer, is two-dimensional structure material, its table in mechanics, optics, calorifics and electricity
Reveal good property.In carbon-based material, graphene is with its unique architectural characteristic and excellent performance and production cost
Relative moderate, graphene is set to be applied in many field of scientific studies.The graphene of individual layer is reunited in a solvent, and dispersiveness is not
It is good, therefore the functionalization of graphene and dispersiveness are most important in the application.Chemistry functional graphene is avoided that mono-layer graphite
Alkene solvent phase reunion, and largely retain graphene essence.Contain substantial amounts of hydroxyl, carboxyl and ring on graphene oxide
Oxygen isoreactivity functional group, the presence of these oxygen-containing functional groups, surface modification is carried out to graphene oxide using chemical reaction, makes it
Effective interface cohesion is formed between polymeric matrix, reaches dispersed in the polymer.
Show at present on mechanically polishing the result of study of retaining ring, polyether-ether-ketone composite material is current preparation retaining ring
Ideal material, it can meet the performance requirements of retaining ring, and can improve the wear-out life of retaining ring.
The content of the invention
Protected it is an object of the invention to provide a kind of polyether-ether-ketone wearing composite material, preparation method and its in mechanical polishing
Applied in terms of held in ring.
A kind of polyether-ether-ketone wearing composite material of the present invention, by polyether-ether-ketone resin and coupling agent modified oxidation
Graphene forms, and is calculated by quality 100%, and the weight/mass percentage composition of polyether-ether-ketone resin is 90~99.99%, and remaining is coupling
The graphene oxide that agent is modified.
Further, the melt index of described polyether-ether-ketone resin is that 20~25g/10min (is referred to by XRZ-400 meltings
Number instrument measure, test condition：400 DEG C, load dispel code weight 5kg, polymer load test barrel preheating 5min), polyether-ether-ketone powder
Last 10~20um of particle diameter.
Further, described graphene oxide is prepared using improved Hummers methods, including pre-oxidizes and aoxidize two
Step,
Pre-oxidation：2.0~3.0g potassium peroxydisulfates and 1.0~3.0g phosphorus pentoxides are added to 10~15mL concentrated sulfuric acids
In (mass fraction be 96~98%), being stirred and heated to 75~95 DEG C makes its dissolving, add 2~5g graphite powders continue 75~
5~7h of stirring reaction under the conditions of 95 DEG C；Room temperature is down to after reaction completely, adds the dilution of 400~600mL deionized waters, filters, use
Absolute ethyl alcohol washing, dry, obtain pre-oxidizing graphite；
Oxidation：Above-mentioned pre-oxidation graphite is added to the concentrated sulfuric acid of 60~100mL ice baths (mass fraction is 96~98%)
In, 6~10g potassium permanganate is slowly added to, temperature control is below 10 DEG C；Be warming up to after addition 30~40 DEG C reaction 1~
3h, be slow added into 100~200mL deionized waters, continue to add after 0.5~1h of stirring 500~700mL deionized waters and 5~
15mL hydrogen peroxide (mass fraction 30%)；Finally above-mentioned solution is filtered, with the salt acid elution of mass fraction 8~15%,
Washed to neutrality, dried with absolute ethyl alcohol again, added deionized water 0.5~1.5h of ultrasound afterwards, be made into 5~10mg/mL oxygen
Graphite aqueous dispersions, dialyse 2~5 days, then by 25~35min of above-mentioned graphite oxide solution ultrasonic disperse, filter, with anhydrous second
Alcohol washing, obtain graphene oxide after drying.
A kind of preparation method of polyether-ether-ketone wearing composite material, its step are as follows：
A. coupling agent modified graphene oxide：0.1~0.8g graphene oxides are taken to be added to 10~100mL absolute ethyl alcohols
In solution (mass fraction >=99.7%), be stirred by ultrasonic 20~40min, by 0.5~3.5mL silane couplers (KH550 or
DB551) it is added drop-wise in above-mentioned solution, 5~15h is reacted under the conditions of 65~85 DEG C, is dried after filtering, washing, obtains coupling agent
Modified graphene oxide；
B. in ethanol solution, concentration is coupling agent modified graphene oxide ultrasonic disperse step A obtained
0.05~0.50g/10mL, jitter time are 0.5~2h；
C. the coupling agent modified graphene oxide after ultrasonic disperse step B obtained is scattered in polyether-ether-ketone powder
In absolute ethyl alcohol, 10~30min of ultrasonic disperse, then the mechanical mixture through 20~30min at normal temperatures, filter after 60~80 DEG C
Under the conditions of dry 6~8h；
D. the dried mixtures of step C are added in double screw extruder, be kneaded under conditions of 360~380 DEG C,
Extrusion, it is granulated, dries, then melting dried pellet in injection machine, injects mould molding, it is wear-resisting to obtain polyether-ether-ketone
Composite.
Polyether-ether-ketone wearing composite material prepared by the present invention can be applied in terms of retaining ring is mechanically polished.Changing
Learn in mechanical polishing operation, add a retaining ring in wafer periphery, can so alleviate the stress concentration of crystal round fringes, so as to
Solve crystal column surface unbalance stress and cause " overground " phenomenon of crystal round fringes, make crystal column surface life that there is close flatness tolerance
Uniform polish surface.Specifically polyether-ether-ketone wearing composite material is prepared into and keeps ring-like, as shown in Fig. 2 in retaining ring
Footpath is 301mm, and external diameter is 345mm, and thickness is 7.05mm.
Compared with pure polyether-ether-ketone resin, the present invention is using the coupling agent modified oxygen that wearability is good, self lubricity is good
Graphite alkene carries out surface modification treatment to strengthen itself and polyether-ether-ketone matrix compatibility as filler to it, carries simultaneously
High interface interaction power between packing material and matrix.Relatively low coefficient of friction is possessed compared to pure polyether-ether-ketone by friction testing
And wear rate.The good self lubricity of graphene oxide itself is taken full advantage of, and also illustrate that coupling agent modified oxidation
Graphene has good compatibility with polyether-ether-ketone matrix.Due in the base dispersiveness and good interface compatibility, rubbing
During, be advantageous to stabilization, homogeneous transfer membrane is formed, reduce the roughness in friction pair face, reduce coefficient of friction and mill
Loss rate.
The service life wear rate low by uniform surface for mechanically polishing retaining ring determined, polyether-ether-ketone of the invention
Wearing composite material can meet the critical demands of retaining ring processing, including intensity, heat resistance and polishing fluid composition compatibility.
Brief description of the drawings
Fig. 1 is the scanning of the coupling agent modified graphene oxide prepared using improved Hummers methods of the present invention
Electron microscopic picture；
As can be seen from the figure coupling agent modified surface of graphene oxide has many fold patterns, illustrates in oxidizing process
Middle graphite flake layer is opened well；
Fig. 2 is the mechanical polishing retaining ring structural representation of the polyether-ether-ketone composite material of the present invention.
Light grey annulus is to be circularized by polyether-ether-ketone composite material by injection molding technology to inject in figure, ring
Shape internal diameter is 300mm, and external diameter is 345mm, and thickness is 7.05mm.
Embodiment
Technical scheme is illustrated below by specific embodiment, described embodiment is simply to the present invention
Claim specific descriptions, claim includes but is not limited to described embodiment content.
Embodiment 1
First, graphene oxide is prepared using improved hummers methods, detailed process is as follows：
Pre-oxidation：2.5g potassium peroxydisulfates and 2.5g phosphorus pentoxides are added to the 12mL concentrated sulfuric acids (mass fraction 98%)
In, being stirred and heated to 80 DEG C makes its dissolving, adds 3g graphite powders and continues in 80 DEG C of stirring reaction 6h.Room is down to after reaction completely
Temperature, 0.5L deionized waters are added, filter, be washed till neutrality with absolute ethyl alcohol afterwards, 8h is dried at 65 DEG C, obtain pre-oxidizing stone
Ink.
Oxidation：Above-mentioned pre-oxidation graphite is added in the concentrated sulfuric acid (mass fraction 98%) of 80mL ice baths, is slowly added to
8g potassium permanganate, temperature control is at 5 DEG C.After adding, 35 DEG C of reaction 3h are warming up to, 150mL deionized waters is slowly added to, stirs
500mL deionized waters and 10mL hydrogen peroxide (mass fraction 30%) are added after 0.5h.Above-mentioned solution is filtered, uses matter
Measure the salt pickling of fraction 10%, after washed with absolute ethyl alcohol to neutrality, in 65 DEG C of drys 6h, it is ultrasonic to add deionized water afterwards
1h, is made into about 5mg/mL graphite oxide aqueous dispersions, dialyses 3 days, then ultrasonic disperse 30min, after suction filtration, uses absolute ethyl alcohol
Washing, graphene oxide is obtained in 80 DEG C of dry 10h.
Surface modification treatment：Take 0.10g graphene oxides to be added in 15mL ethanol solutions, 30min be stirred by ultrasonic,
0.5mL Silane coupling agent KH550s are added drop-wise in above-mentioned solution, 10h is reacted at 75 DEG C, dries, is coupled after filtering, washing
The graphene oxide 0.12g that agent is modified.
By coupling agent modified graphene oxide 0.05g ultrasonic disperses in 10mL ethanol solutions, concentration is
0.05g/10mL, jitter time 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, 10~20um of powder diameter) powder
49.95g ultrasonic disperses disperse the mechanical mixture through 30min at normal temperatures after 30min in 500mL ethanol solutions, filter
After 80 DEG C of dry 8h；
Above-mentioned dried mixture is added in double screw extruder, is kneaded, extrudes under conditions of 380 DEG C, make
Grain, and pellet is dried, dried pellet is melted in injection machine, is injected separately into bending, stretching or friction mould molding,
Obtain polyether-ether-ketone composite material test bars.Tensile bars are dumbbell shape, and size is 4.0 × 9.0 × 40.0mm, bend batten
Size is 4.0 × 6.0 × 55.0mm, and friction batten is diameter 6.3mm, height 18.8mm cylindrical batten.
Embodiment 2
Graphene oxide preparation process and step in the present embodiment take improved hummers method systems in embodiment 1
Standby graphene oxide process；
Surface modification treatment：Take 0.30g graphene oxides to be added in 45mL ethanol solutions, 30min be stirred by ultrasonic,
1.5mL Silane coupling agent KH550s are added drop-wise in above-mentioned solution, 10h is reacted at 75 DEG C, dries, is coupled after filtering, washing
The graphene oxide 0.34g that agent is modified.
Coupling agent modified graphene oxide 0.25g is dispersed in 10mL anhydrous ethanol solvents, concentration 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 ethanol solutions, after ultrasonic disperse 30min
Mechanical mixture through 20min at normal temperatures, filter after 80 DEG C of dry 8h；
Above-mentioned dried mixture is added in double screw extruder, is kneaded, extrudes under conditions of 380 DEG C, make
Grain, and pellet is dried, dried pellet is melted in injection machine, mould molding is injected, obtains polyether-ether-ketone composite wood
Expect test sample.
Embodiment 3
Graphene oxide preparation process and step in the present embodiment take improved hummers method systems in embodiment 1
Standby graphene oxide process.
Surface modification treatment：Take 0.60g graphene oxides to be added in 90mL ethanol solutions, 30min be stirred by ultrasonic,
3.0mL Silane coupling agent KH550s are added drop-wise in above-mentioned solution, 10h is reacted at 75 DEG C, dries, is coupled after filtering, washing
The graphene oxide 0.68g that agent is modified.
Coupling agent modified graphene oxide 0.50g is taken to be dispersed in 10mL anhydrous ethanol solvents, concentration 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 ethanol solutions, after ultrasonic disperse 30min
Mechanical mixture through 30min at normal temperatures, filter after 80 DEG C of dry 8h；
Above-mentioned dried mixture is added in double screw extruder, is kneaded, extrudes under conditions of 380 DEG C, make
Grain, and pellet is dried, dried pellet is melted in injection machine, mould molding is injected, obtains polyether-ether-ketone composite wood
Expect test sample.
After polyether-ether-ketone composite material made from embodiment 1,2,3 is processed into test bars by injecting mould molding,
According to the requirement of following table test condition, material friction wear properties test is carried out, it is as a result 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 of embodiment 3
Polishing machine is optimal, is 1MPa in load, testing time 2h, and test speed is under 200r/min DRY SLIDING, and pure
Material reduces 6.5% compared to coefficient of friction, and wear rate reduces 29%.
As can be seen from Table 2 the tensile strength of embodiment 1~3 and elongation at break relative to pure polyether-ether-ketone
Lifting, tensile strength embodiment 1~3 improve 13.2%, 14.0%, 13.5% respectively, and elongation at break improves respectively
23.4%th, 41.0%, 4.8%.Bending strength is not lifted compared with pure polyether-ether-ketone.
Table 1：Polyether-ether-ketone composite material polishing machine test result
Note：Friction and wear behavior is using UMT-2 (Bruker, Germany) test, according to ASTMG99-04 standards.
Table 2：Polyether-ether-ketone composite material mechanical experimental results
Claims (4)
1. a kind of preparation method of polyether-ether-ketone wearing composite material, its step are as follows：
1) by coupling agent modified graphene oxide ultrasonic disperse in ethanol solution, concentration is 0.05~0.50g/
10mL, jitter time are 0.5~2h；
2) the coupling agent modified graphene oxide after the ultrasonic disperse for obtaining step 1) is scattered in nothing with polyether-ether-ketone powder
In water-ethanol, 10~30min of ultrasonic disperse, then the mechanical mixture through 20~30min at normal temperatures, filter after 60~80 DEG C of bars
6~8h is dried under part；
3) the dried mixture of step 2) is added in double screw extruder, is kneaded, squeezes under conditions of 360~380 DEG C
Go out, be granulated, drying, then melting dried pellet in injection machine, injecting mould molding, it is wear-resisting multiple to obtain polyether-ether-ketone
Condensation material；
Wherein, described polyether-ether-ketone wearing composite material, it is by polyether-ether-ketone resin and coupling agent modified graphene oxide
Composition, calculated by quality and 100%, the weight/mass percentage composition of polyether-ether-ketone resin is 90~99.99%, and remaining changes for coupling agent
The graphene oxide of property；Coupling agent modified graphene oxide be take 0.1~0.8g graphene oxides be added to 10~100mL without
In hydrous ethanol solution, 20~40min is stirred by ultrasonic, then 0.5~3.5mL silane couplers are added drop-wise in above-mentioned solution,
5~15h is reacted under the conditions of 65~85 DEG C, dries and is prepared after filtering, washing.
A kind of 2. preparation method of polyether-ether-ketone wearing composite material as claimed in claim 1, it is characterised in that：Graphite oxide
Alkene is that 2.0~3.0g potassium peroxydisulfates and 1.0~3.0g phosphorus pentoxides are added in 10~15mL concentrated sulfuric acids, is stirred and heated to
75~95 DEG C make its dissolving, add 2~5g graphite powders and continue 5~7h of stirring reaction under the conditions of 75~95 DEG C；Reaction is complete
After be down to room temperature, add the dilution of 400~600mL deionized waters, filter, washed with absolute ethyl alcohol, dry, obtain pre-oxidizing stone
Ink；Pre-oxidation graphite is added in the concentrated sulfuric acid of 60~100mL ice baths again, is slowly added to 6~10g potassium permanganate, temperature control
System is below 10 DEG C；30~40 DEG C of 1~3h of reaction are warming up to after addition, are slow added into 100~200mL deionized waters,
500~700mL deionized waters and 5~15mL hydrogen peroxide are added after continuing 0.5~1h of stirring；Finally above-mentioned solution is filtered,
With the salt acid elution of mass fraction 5~15%, then with absolute ethyl alcohol wash to it is neutral, dry, add deionized water ultrasound afterwards
0.5~1.5h, 5~10mg/mL graphite oxide aqueous dispersions are made into, dialysed 2~5 days, then above-mentioned graphite oxide solution is surpassed
Sound disperses 25~35min, filters, is washed with absolute ethyl alcohol, obtains graphene oxide after drying.
A kind of 3. preparation method of polyether-ether-ketone wearing composite material as claimed in claim 1, it is characterised in that：It is silane coupled
Agent is KH550 or DB551.
4. polyether-ether-ketone wearing composite material prepared by claim 1,2 or 3 methods describeds is in terms of retaining ring is mechanically polished
Using.
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| CN106633626B (en) * | 2016-09-27 | 2019-03-22 | 广东银禧科技股份有限公司 | Graphene/polyether-ether-ketone composite powder material and preparation method for SLS |
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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 |
| 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 |
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