CN108517104A - A kind of polyether-ether-ketone composite material and preparation method thereof - Google Patents
A kind of polyether-ether-ketone composite material and preparation method thereof Download PDFInfo
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/22—Oxides; Hydroxides of metals
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- C08K2003/2241—Titanium dioxide
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Abstract
The present invention discloses a kind of polyether-ether-ketone composite material, is made of the raw material of following weight percent：Polyether-ether-ketone 90~96%, nanometer diamond alkene 1~3%, nano-titanium dioxide P25 1~7%.There is provided its corresponding preparation method simultaneously.It is added to nanometer diamond alkene and nano-titanium dioxide P25 in the trielement composite material of the present invention, nanometer diamond alkene has no toxic side effect to human body, nanometer diamond alkene hardness is high, wearability is strong, stability is high, the friction factor of composite material can be reduced, wear rate, nanometer diamond alkene and nano-titanium dioxide P25 are in the composite, reducing friction factor, synergistic effect is played in terms of wear rate, trielement composite material friction factor obtained is low, low wear rate, reduce the abrasion to material, extend the service life of wear-resistant material, thermal stability is high, it can meet and be used under high temperature harsh environment, expand the application of PEEK.
Description
Technical field
The invention belongs to engineering material technical fields, and in particular to a kind of polyether-ether-ketone composite material and preparation method thereof.
Background technology
In human social activity, mainly there are fretting wear, fracture, corrosion etc. in the reason of material failure, and fretting wear
Lead to spillage of material accounts for 50%, i.e., the part energy is not utilized has just wasted.Furthermore there are security risk, examples for friction behavior
Such as, in mine, frictional heat and spark may cause on fire, or even explosion, cause the accident and lose；It is led in auto-parts
The damage in domain, engine, damper, brake etc. is mainly caused by friction, if things go on like this, may lead to motor vehicle liquidation；
Aerospace field causes poorly sealed or generates spark by reasons such as not corrosion-resistant and frictions, and then fuel explodes
Event, it is commonplace, cause greatly property loss.
After entering the new century, as social progress, economic productivity develop, friction material also urgently development and application,
And all trades and professions are to rub resistance material that more stringent requirements are proposed, for example, wearability enhancing, corrosion-resistant, application range is wide, stablizes
Property equal aspect of performance by force requirement.Currently, Polymer Friction Materials have been due to having dominated the market gradually with excellent performance, by
It walks instead of the friction device part for using metal material to prepare before.
Polyether-ether-ketone (PEEK) is a kind of semi-crystalline thermoplastic's special engineering plastics of high comprehensive performance, and commercialization
Poly aryl ether ketone in most widely used, most mainstream product, main chain is made of phenyl ring, ehter bond, carbonyl, and structural formula is as follows.
For polyether-ether-ketone as a kind of hemicrystalline fire resistant resin, maximum crystallinity is 48%, commonly uses the crystallinity of product
It is 20%~30%, glass transition temperature TgIt is 143 DEG C, fusing point TmIt is 343 DEG C, mainly there are following excellent properties：
1, heat resistance is good, be used for a long time temperature can reach 250 DEG C, even at 300 DEG C also can short-term operation,
Its heat resistance is far above resins such as makrolon, ABS；
2, mechanical property is good, and polyether-ether-ketone has high modulus and intensity, can compare favourably with thermosets, simultaneously
Also there is good toughness, impact resistance, fatigue durability, good combination property to be conducive to extend the service life of part；
3, good stability of the dimension contains a large amount of phenyl ring in the strand of polyether-ether-ketone, and rigidity is strong, and product has good
Dimensional stability, coefficient of thermal expansion is small；
4, good wear-resisting property, polyether-ether-ketone have self lubricity, have lower friction coefficient and wear extent；
5, good flame retardant property, polyether-ether-ketone have self-extinguishment, compound stringent safety requirements；
6, good solvent resistance, the stable chemical performance of polyether-ether-ketone are practically insoluble in other in addition to the concentrated sulfuric acid
Any soda acid or organic reagent, corrosion resistance are fabulous；
7, electrical insulating property, dielectric constant are 3.2~3.3, and at 1KHz, dielectric loss is 0.0016, and breakdown voltage is
17KV/mm, are-tight property are 175V, can be used as C class F insulating material Fs, while electrical insulation capability stabilization, not with temperature, wet
Degree, power frequency variation and change；
8, excellent processing performance, polyether-ether-ketone itself are thermoplastic resins, can carry out secondary operation, good fluidity,
It is readily extruded and injection molding, shaping efficiency is high.
Therefore, have in fields such as space flight, military affairs, industry, the energy and widely apply.
But currently, the requirement to rub resistance material is higher and higher, in order to remain to normally make in harsh working environment
With for example, under top load, high sliding speed, hot conditions, material must also keep low-friction coefficient and wear extent, and polyethers
Therefore the requirement that ether ketone resin cannot meet under harsh work is changed commanders need to be modified polyether-ether-ketone, to reduce it
Friction coefficient and wear extent widen the application range of polyether-ether-ketone.
Invention content
Present invention aims at a kind of polyether-ether-ketone composite materials of offer, while it is this hair to provide its corresponding preparation method
Bright another goal of the invention.
Based on above-mentioned purpose, the present invention takes following technical scheme：
A kind of polyether-ether-ketone composite material is made of the raw material of following weight percent：Polyether-ether-ketone 90~96%, nanometer
Diamond alkene 1~3%, nano-titanium dioxide P25 1~7%.
The nanometer diamond alkene is made of the nanometer diamond alkene that granularity is 50nm, 100nm, 200nm, 250nm, 50nm,
The mass ratio of the nanometer diamond alkene of 100nm, 200nm, 250nm is (1~2) ︰ (2~3) ︰ (3~4) ︰ (4~5).
The method for preparing polyether-ether-ketone composite material, includes the following steps：
1) it is that (1~3) ︰ (1~7) ratio mixes, and obtains mixed according to mass ratio by nanometer diamond alkene, nano-titanium dioxide P25
Close object A；
2) in supersonic frequency is 40~60KHz, speed of agitator is to mix deionized water and step 1) under 30~60rpm
Object A is stirred 25-35min, at 65-75 DEG C, then proceedes to that 3-aminopropyltriethoxysilane is added, reacts 3-4h,
Centrifugation, will centrifugation product drying, heat treatment, cooling modified mixture B, deionized water, three second of mixture A and 3- aminopropyl
The amount ratio of oxysilane is 100mL ︰ 1g ︰ 6mL；
3) by step 2) modified mixture B and polyether-ether-ketone mixing, melting extrusion, drying, injection molding, polyether-ether-ketone is obtained
Composite material.
Step 2) centrifugal condition：Centrifugal rotational speed is 4000~8000rpm, centrifugation time is 10~15min；Drying condition：
Drying temperature is 60~80 DEG C, drying time is 4~12h.
Heat treatment takes level Four staged to heat up in step 2), after first stage temperature rises to 60 DEG C by room temperature, heat preservation
30min；After second stage temperature rises to 120 DEG C by 60 DEG C, 1h is kept the temperature；After phase III temperature rises to 280 DEG C by 120 DEG C, protect
Warm 3h；After fourth stage temperature rises to 400 DEG C by 280 DEG C, 10h is kept the temperature, during each step-up temperature, heating rate is 2~3
℃/min。
When modified mixture B and polyether-ether-ketone mix in step 3), it is placed in SHR high-speed mixers, is in power of agitator
Under 42KW, speed of agitator 1050rpm, 6~10min is stirred.
Minipool rheometer is taken in step 3) melting extrusion, and processing temperature is 370 DEG C~395 DEG C, screw speed 50
~80rpm；Step 3) drying condition：Drying temperature is 120 DEG C, drying time 10h.
When step 1) nanometer diamond alkene, nano-titanium dioxide P25 mixing, it is placed in SHR high-speed mixers, in power of agitator
Under 42KW, speed of agitator 1050rpm, to stir 6~10min.
Compared with prior art, the invention has the advantages that：
Advantages of the present invention：
1, nanometer diamond alkene and nano-titanium dioxide P25, nanometer diamond alkene are added in trielement composite material of the invention
Have no toxic side effect to human body, nanometer diamond alkene hardness is high, wearability is strong, and stability is high, can reduce the friction of composite material because
Number, wear rate, nanometer diamond alkene and nano-titanium dioxide P25 in the composite, rise in terms of reducing friction factor, wear rate
Synergistic effect is arrived, trielement composite material friction factor obtained is low, low wear rate, reduces the abrasion to material, extends
The service life of wear-resistant material, thermal stability is high, can meet and be used under high temperature harsh environment, expand the application of PEEK；
2, preparation method is simple, easy to operate, and device therefor is few, and production cost is low.
Description of the drawings
Fig. 1 is different nano-titanium dioxide P25 additive amounts to TiO2The friction coefficient of/PEEK composite materials influences；
Fig. 2 is different nano-titanium dioxide P25 additive amounts to TiO2The wear rate of/PEEK composite materials influences；
Fig. 3 is influence of the different nanometer diamond alkene additive amounts to NA/PEEK composite material friction factors；
Fig. 4 is influence of the different nanometer diamond alkene additive amounts to the wear rate of NA/PEEK composite materials；
Fig. 5 is nano-titanium dioxide P25 to TiO2The influence of the Vickers hardness of/PEEK composite materials；
Fig. 6 is influence of the nanometer diamond alkene to NA/PEEK composite material Vickers hardnesses.
Specific implementation mode
Embodiment 1
A kind of polyether-ether-ketone composite material is made of the raw material of following weight percent：Polyether-ether-ketone 96%, nanometer diamond
Alkene 1%, nano-titanium dioxide P25 3%.
The nanometer diamond alkene is made of the nanometer diamond alkene that granularity is 50nm, 100nm, 200nm, 250nm, 50nm,
The mass ratio of the nanometer diamond alkene of 100nm, 200nm, 250nm is 1 ︰, 2 ︰, 3 ︰ 4.
The method for preparing polyether-ether-ketone composite material, includes the following steps：
1) it is that 1 ︰, 3 ratios are placed in SHR high-speed mixers according to mass ratio by nanometer diamond alkene, nano-titanium dioxide P25,
It is to stir 10min under 42KW, speed of agitator 1050rpm, obtain mixture A in power of agitator；
2) in supersonic frequency is 40KHz, speed of agitator is under 30rpm, by 100mL deionized waters and 1g step 1) mixtures
A is stirred 30min, continues to stir, dropwise instill 6mL 3-aminopropyltriethoxysilane, reaction temperature be 70 DEG C at,
4h is reacted, it is to centrifuge 15min under 4000rpm to be then centrifuged for rotating speed, at 60 DEG C, by centrifugation product (predominantly nanometer diamond alkene
With nano-titanium dioxide P25) drying 12h, high-temperature heat treatment, natural cooling obtain modified mixture B；High-temperature heat treatment takes four
Grade staged heating, after first stage temperature rises to 60 DEG C by room temperature, keeps the temperature 30min；Second stage temperature rises to 120 by 60 DEG C
After DEG C, 1h is kept the temperature；After phase III temperature rises to 280 DEG C by 120 DEG C, 3h is kept the temperature；Fourth stage temperature rises to 400 by 280 DEG C
After DEG C, 10h is kept the temperature, during each step-up temperature, heating rate is 2 DEG C/min,
3) step 2) modified mixture B and polyether-ether-ketone are placed in SHR high-speed mixers, in power of agitator be 42KW,
Under speed of agitator 1050rpm, 10min is stirred, processing temperature is 395 DEG C, screw speed is to take minipool stream under 50rpm
Become instrument (HAAKE MiniLab, match silent winged generation that science and technology, and screw rod rotates for conical parallel dual) and carry out melting extrusion, is placed in 120 DEG C of bakings
In case, dry 10h, using micro-injection forming instrument (HAAKE MiniJet match silent winged generation that science and technology) injection molding, condition is：
Barrel temperature is 395 DEG C, and mould-cavity temperature is 180 DEG C, injection pressure 900bar, retention time 20s, dwell pressure 700bar, is protected
Time 20s is pressed, at 200 DEG C, constant temperature is heat-treated 2h, is annealed to room temperature, obtains polyether-ether-ketone composite material.
Embodiment 2
A kind of polyether-ether-ketone composite material is made of the raw material of following weight percent：Polyether-ether-ketone 94%, nanometer diamond
Alkene 1%, nano-titanium dioxide P25 5%.
The nanometer diamond alkene is made of the nanometer diamond alkene that granularity is 50nm, 100nm, 200nm, 250nm, 50nm,
The mass ratio of the nanometer diamond alkene of 100nm, 200nm, 250nm is 1 ︰, 2 ︰, 3 ︰ 4.
The method of polyether-ether-ketone composite material is prepared with reference to embodiment 1.
Embodiment 3
A kind of polyether-ether-ketone composite material is made of the raw material of following weight percent：Polyether-ether-ketone 95%, nanometer diamond
Alkene 2%, nano-titanium dioxide P25 3%.
The nanometer diamond alkene is made of the nanometer diamond alkene that granularity is 50nm, 100nm, 200nm, 250nm, 50nm,
The mass ratio of the nanometer diamond alkene of 100nm, 200nm, 250nm is 1 ︰, 2 ︰, 3 ︰ 4.
The method of polyether-ether-ketone composite material is prepared with reference to embodiment 1.
Embodiment 4
A kind of polyether-ether-ketone composite material is made of the raw material of following weight percent：Polyether-ether-ketone 90%, nanometer diamond
Alkene 3%, nano-titanium dioxide P25 7%.
The nanometer diamond alkene is made of the nanometer diamond alkene that granularity is 50nm, 100nm, 200nm, 250nm, 50nm,
The mass ratio of the nanometer diamond alkene of 100nm, 200nm, 250nm is 2 ︰, 3 ︰, 4 ︰ 5.
The method for preparing polyether-ether-ketone composite material, includes the following steps：
1) it is that 3 ︰, 7 ratios are placed in SHR high-speed mixers according to mass ratio by nanometer diamond alkene, nano-titanium dioxide P25,
It is to stir 6min under 42KW, speed of agitator 1050rpm, obtain mixture A in power of agitator；
2) in supersonic frequency is 60KHz, speed of agitator is under 60rpm, by 100mL deionized waters and 1g step 1) mixtures
A is stirred 30min, continues to stir, and instills 6mL3- aminopropyltriethoxywerene werenes dropwise, and reaction temperature is at 70 DEG C, instead
4h is answered, it is to centrifuge 10min under 8000rpm to be then centrifuged for rotating speed, is (predominantly to receive centrifugation product at 60 DEG C in drying temperature
Rice diamond alkene and nano-titanium dioxide P25) drying 4h, high-temperature heat treatment, natural cooling obtain modified mixture B；High-temperature heat treatment
It takes level Four staged to heat up, after first stage temperature rises to 60 DEG C by room temperature, keeps the temperature 30min；Second stage temperature is by 60 DEG C
After rising to 120 DEG C, 1h is kept the temperature；After phase III temperature rises to 280 DEG C by 120 DEG C, 3h is kept the temperature；Fourth stage temperature is by 280 DEG C
After rising to 400 DEG C, 10h is kept the temperature, during each step-up temperature, heating rate is 3 DEG C/min,
3) step 2) modified mixture B and polyether-ether-ketone are placed in SHR high-speed mixers, in power of agitator be 42KW,
Under speed of agitator 1050rpm, 6min is stirred, processing temperature is 370 DEG C, screw speed is to take minipool rheology under 50rpm
Instrument (HAAKE MiniLab, matching silent winged generation, you are scientific and technological, and screw rod rotates for conical parallel dual) carries out melting extrusion, is placed in 120 DEG C of baking ovens
In, dry 10h, using micro-injection forming instrument (HAAKE MiniJet match silent winged generation that science and technology) injection molding, condition is：Material
Cylinder temperature is 380 DEG C, and mould-cavity temperature is 180 DEG C, injection pressure 900bar, retention time 20s, dwell pressure 700bar, pressurize
Time 20s, at 200 DEG C, constant temperature is heat-treated 2h, is annealed to room temperature, obtains polyether-ether-ketone composite material.
Embodiment 5
A kind of polyether-ether-ketone composite material is made of the raw material of following weight percent：Polyether-ether-ketone 92%, nanometer diamond
Alkene 2%, nano-titanium dioxide P25 6%.
The nanometer diamond alkene is made of the nanometer diamond alkene that granularity is 50nm, 100nm, 200nm, 250nm, 50nm,
The mass ratio of the nanometer diamond alkene of 100nm, 200nm, 250nm is 2 ︰, 3 ︰, 4 ︰ 5.
The method of polyether-ether-ketone composite material is prepared with reference to embodiment 4.
6 performance test of embodiment
The hardness test of composite material
Using composite sample after injection molding, surface is smooth, cylindrical, diameter 15mm, height 1.5mm,
Hardness test is carried out using electronic digital display vickers hardness tester (MHV-30Z), test condition is：Load 2Kg, pressurize 15s, each sample
Product test ten groups of panel datas, take its average value.
The tribology behavior of composite material characterizes
Composite sample after injection molding, cylindrical, diameter 6.3mm, height 18.8mm are tried using Multifunctional friction
Machine (German UMT-2, Bruker) is tested, according to ASTM G99-04 standards, pin-disc type contact type is unidirectional to slide, and friction pair is
45#Stainless steel (diameter 50mm, height 10mm) all uses different roughness (900 before test every time#With 1500#) waterproof abrasive paper to sample
Product surface and the secondary steel disk surface sanding and polishing of friction, then be cleaned by ultrasonic with acetone, the sample and steel disk that sanding and polishing is crossed, drying is cold
But, initial weight m is weighed with electronic digital display balance1, after completing tribology tester, it is cleaned by ultrasonic sample with acetone again, it is dry
The example weight m after test is weighed after cooling2.In order to investigate friction scholarship and moral conduct of the composite material under different loads and sliding speed
For test condition is respectively 2MPa (62.32N), 200rpm (0.42m/s)；2MPa (62.32N), 400rpm (0.84m/s)；
4MPa (124.64N), 200rpm (0.42m/s).The testing time of each sample is 2h, and every group at least takes three groups of panel datas
Average value.
The friction factor of composite material changes over time curve and carries software records by instrument, and wear rate formula the following is：
Wherein：Volume erosion rate (the mm of Ws- composite materials3/ Nm), m1The quality (g) of sample, m before friction testing2-
The quality (g) of sample after friction testing, the density (g/cm of ρ-sample3), F- friction testings apply load (N), L- friction testings
Total coasting distance (m),
Density p surveys density principle with drainage, is tested using electronic digital display densitometer (Mettler SD-200L).
The thermal stability of composite material
The thermal stability that composite material is investigated using thermogravimetric analyzer (Pyris 1 TGA, Perkin Elmer), is learnt from else's experience dry
Dry extrusion 3~5mg of pellet, measurement atmosphere are nitrogen, constant temperature 10min at 100 DEG C, then are heated up with the heating rate of 10 DEG C/min
To 800 DEG C, the heat decomposition temperature T of weightlessness 5% is calculated according to obtained thermogravimetric curve5%.
Every group of test sample constituent is (raw material page 7) as shown in table 1 below, and NA is nanometer diamond alkene.
1 test sample constituent table of table
| Sample | PEEK (wt%) | NA (wt%) | TiO2(wt%) |
| PEEK | 100 | 0 | 0 |
| 1%NA/PEEK | 99 | 1 | 0 |
| 1.5%NA/PEEK | 98.5 | 1.5 | 0 |
| 2%NA/PEEK | 98 | 2 | 0 |
| 2.5%NA/PEEK | 97.5 | 2.5 | 0 |
| 3%NA/PEEK | 97 | 3 | 0 |
| 1%TiO2/PEEK | 99 | 0 | 1 |
| 3%TiO2/PEEK | 97 | 0 | 3 |
| 5%TiO2/PEEK | 95 | 0 | 5 |
| 7%TiO2/PEEK | 93 | 0 | 7 |
| 1%NA/3%TiO2/PEEK | 96 | 1 | 3 |
| 1%NA/5%TiO2/PEEK | 94 | 1 | 5 |
| 2%NA/3%TiO2/PEEK | 95 | 2 | 3 |
In order to determine the optimum filling amount of nanometer diamond alkene and nano-titanium dioxide P25 in polyether-ether-ketone matrix, first
The friction and wear behavior for having investigated nano-titanium dioxide P25 and the single filling-modified PEEK composite materials of nanometer diamond alkene carries out
Shadow of the different loadings to the friction and wear behavior of PEEK composite materials (preparation method is with reference to embodiment 1) has been investigated in research
It rings, while having investigated under different friction environment (different loads, different sliding speeds), PEEK composite materials friction factor and mill
The situation of change of loss rate.
6.1 different nano-titanium dioxide P25 additive amounts are to TiO2The influence of the friction and wear behavior of/PEEK composite materials
As shown in Fig. 1, test condition, a：2MPa、200rpm、2h；b：2MPa、400rpm、2h；c：4MPa、200rpm、
2h。
As shown in Figure 1, under different experimental conditions, when the content of nano-titanium dioxide P25 is in 1%~7% range
When, TiO2The friction factor of/PEEK composite materials, which shows, first to be reduced, rear raised trend, 3%TiO2/ PEEK composite material tables
Best tribology behavior is revealed, friction factor is minimum.Under conditions of 2MPa, 200rpm, nano-titanium dioxide is not contained
The friction factor of the pure PEEK materials of P25 is about 0.433, with the increase of nano-titanium dioxide P25 additive amounts, friction factor by
Gradually reduce, when nano-titanium dioxide P25 additive amounts are 1%, 1%TiO2The friction factor about 0.422 of/PEEK composite materials, drop
Low about 2.54%；When nano-titanium dioxide P25 additive amounts are 3%, 3%TiO2The friction factor of/PEEK composite materials is minimum,
About 0.4057, reduce about 6.3%；When nano-titanium dioxide P25 additive amounts are 5%, 5%TiO2/ PEEK composite materials
Friction factor rises, and about 0.424, reduce about 2.07%；When nano-titanium dioxide P25 additive amounts are 7%, 7%TiO2/
The friction factors of PEEK composite materials rises, and about 0.43, it rubs substantially with the pure PEEK of no addition nano-titanium dioxide P25
It is identical to wipe factor.
After load or sliding speed increase, TiO2The friction factor of/PEEK composite materials, which also shows, first to be reduced, rear liter
High trend.In TiO2In/PEEK systems, TiO2/ PEEK composite materials are twice in friction additional load or sliding speed increasing
Afterwards, friction factor increases, with 3%TiO2It is illustrated for/PEEK, when same rotational speed, under 4MPa, friction factor is about
0.432, rise about 6.5%, when same load, under the conditions of 400rpm, friction factor is about 0.43, rises about 6%.
6.2 different nano-titanium dioxide P25 additive amounts are to TiO2The influence of the wear rate of/PEEK composite materials
As shown in Fig. 2, test condition, a：2MPa、200rpm、2h；b：2MPa、400rpm、2h；c：4MPa、200rpm、
2h。
As shown in Figure 2, under different experimental conditions, when the content of nano-titanium dioxide P25 is in 1%~7% range
When, TiO2The wear rate of/PEEK composite materials shows the trend for first dropping and rising afterwards, 3%TiO2The wear rate of/PEEK composite materials
It is minimum.At 2MPa, 200rpm, the wear rate of the pure PEEK materials without containing nano-titanium dioxide P25 is about 4.48mm3/N·
M, with the increase of nano-titanium dioxide P25 additive amounts, wear rate continuously decreases, and nano-titanium dioxide P25 additive amounts are 1%
When, 1%TiO2The wear rate about 3.8mm of/PEEK composite materials3/ Nm reduces about 13.6%；Nano-titanium dioxide P25 adds
When dosage is 3%, 3%TiO2The wear rate of/PEEK composite materials is minimum, about 3.4mm3/ Nm reduces about 22.7%；It receives
When rice titanium dioxide P25 additive amounts are 5%, 5%TiO2The wear rate of/PEEK composite materials rises, about 3.6mm3/ Nm, drop
Low about 18.18%；When nano-titanium dioxide P25 additive amounts are 7%, 7%TiO2The wear rate of/PEEK composite materials rises,
About 5.5mm3/ Nm, the wear rate than the pure PEEK of no addition nano-titanium dioxide P25 is taller, improves about 25%.
After load or sliding speed increase, TiO2The wear rate of/PEEK composite materials also shows first to reduce to be increased afterwards
Trend.In TiO2In/PEEK systems, TiO2/ PEEK composite materials friction additional load or sliding speed increasing be twice after,
Wear rate increases, with 3%TiO2It is illustrated for/PEEK, when same rotational speed, under the conditions of 4MPa, wear rate is about
5.25mm3/ Nm, rises about 53.2%, and when same load, under the conditions of 400rpm, wear rate is about 5.74mm3/ Nm, on
Rise about 67.6%.
Influence of the 6.3 different nanometer diamond alkene additive amounts to NA/PEEK composite material friction factors
As shown in Fig. 3, test condition, a：2MPa、200rpm、2h；b：2MPa、400rpm、2h；c：4MPa、200rpm、
2h。
By such as 3 it is found that under different experimental conditions, when the content of nanometer diamond alkene is in 1%~3% range, NA/
The friction factor of PEEK composite materials, which shows, first rapidly to be reduced, rear slowly raised trend, the loading of nanometer diamond alkene exist
Composite material exhibits have gone out best tribology behavior when in 1%~2% range, and friction factor is minimum.In 2MPa, 200rpm's
Under the conditions of, the friction factor of the pure PEEK materials without containing nanometer diamond alkene is about 0.433, and nanometer diamond alkene additive amount is 1%
When, the friction factor about 0.21 of 1%NA/PEEK composite materials, friction factor rapidly reduces, and reduces about 51.5%；Nanometer is bored
At 1%~2%, the friction factor of NA/PEEK composite materials keeps stablizing stone alkene additive amount, is maintained at 0.21~0.22；It receives
When rice diamond alkene additive amount is 2.5%, the friction factor of 2.5%NA/PEEK composite materials rises, and about 0.25, it reduces about
42.2%；When nanometer diamond alkene additive amount is 3%, the friction factor of 3%NA/PEEK composite materials continues to rise, and about 0.28,
Reduce about 35.3%.
After load or sliding speed increase, the friction factor of NA/PEEK composite materials, which also shows, first rapidly to be reduced, after
Slow raised trend.In NA/PEEK systems, NA/PEEK composite materials increase one in friction additional load or sliding speed
After times, friction factor reduces, and is illustrated by taking 1%NA/PEEK as an example, and when same rotational speed, under the conditions of 4MPa, friction factor is about
It is 0.14, has dropped about 67.6%, when same load, under the conditions of 400rpm, friction factor is about 0.18, is had dropped about
58.4%.
Influence of the 6.4 different nanometer diamond alkene additive amounts to NA/PEEK worn composite rates
As shown in Fig. 4, test condition, a：2MPa、200rpm、2h；b：2MPa、400rpm、2h；c：4MPa、200rpm、
2h。
As shown in Figure 4, under different experimental conditions, when the content of nanometer diamond alkene is in 1%~3% range, NA/
The wear rate of PEEK composite materials, which shows, first rapidly to be reduced, rear slowly raised trend, and the additive amount of nanometer diamond alkene is 1%
When in~2% range, the wear rate of NA/PEEK composite materials is minimum and steady.Under conditions of 2MPa, 200rpm, do not contain
The wear rate of the pure PEEK materials of nanometer diamond alkene is about 4.48mm3/ Nm, with the increase of nanometer diamond alkene additive amount, mill
Loss rate rapidly reduces, when nanometer diamond alkene additive amount is 1%, the wear rate about 1.46mm of 1%NA/PEEK composite materials3/N·
M reduces about 67.4%；When nanometer diamond alkene additive amount is 1.5%, the wear rate of 1.5%NA/PEEK composite materials is about
1.48mm3/ Nm reduces about 66.9%；When nanometer diamond alkene additive amount is 2%, the abrasion of 2%NA/PEEK composite materials
Rate is about 1.5mm3/ Nm reduces about 66.5%.It can be seen that when the additive amount of nanometer diamond alkene is in 1%~2% range
When interior, the low wear rate of NA/PEEK composite materials and steady, when nanometer diamond alkene additive amount is 2.5%, 2.5%NA/PEEK
The wear rate of composite material rises, about 2.2mm3/ Nm reduces about 50.9%, when nanometer diamond alkene additive amount is 3%
When, the wear rate of 2.5%NA/PEEK composite materials continues to rise, about 2.3mm3/ Nm reduces about 48.6%.
After load or sliding speed increase, the wear rate of NA/PEEK composite materials also shows raised after first reducing
Trend.In NA/PEEK systems, NA/PEEK composite materials are after friction additional load or sliding speed increasing are twice, wear rate
It increases, is illustrated by taking 1%NA/PEEK as an example, when same rotational speed, under the conditions of 4MPa, wear rate is about 1.8mm3/ Nm,
Rise about 23.3%, when same load, under the conditions of 400rpm, wear rate is about 1.7mm3/ Nm rises about 16.4%.
The friction factor of composite material is mainly by realistic tribological contact area, material shear strength, material surface energy etc.
The influence of factor,Wherein, μ is friction factor, and F is frictional force, and A is realistic tribological contact area, and P is attached
Lotus is loaded, τ is material shear strength.When additional load or sliding speed increase, it on the one hand can lead to realistic tribological contact surface
Product increases, and frictional heat increases, and friction surface softening increases elasticity and plasticity deformation so that friction factor increases, another party's plane materiel
Softening and micro flow, which occur, for material rubbing surface can reduce the shear strength of material so that friction factor reduces.Nanometer is bored
For stone alkene additive, increases load or sliding speed is equivalent to the severe for increasing friction condition, friction pair can be aggravated
Friction and grinding of the even face steel disk to material surface, fall off as PPEK is rubbed, and more nanometer diamond alkene is caused to expose, by
It is layer structure in nanometer diamond alkene, forms more complete uniform transfer film, play better lubricant effect, show as
Friction factor reduces.For nano-titanium dioxide P25 additives, when nano-titanium dioxide P25 additive amounts are low, nanometer two
Titanium oxide P25 particles can support load on one side, and on the other hand falling off with friction, it is microcosmic rough with paying to be filled into friction
The role between gap, serving as " ball " reduces true friction area, to which friction factor reduces, works as nano-titanium dioxide
When P25 additive amounts are high, as friction falls off, nano-titanium dioxide P25 particles are reunited since specific surface energy is big, are formed big
Grain abrasive accelerates the abrasion to surface so that friction factor and wear rate increase.
By studying nano-titanium dioxide P25 and nanometer diamond alkene respectively as single filler to the frictional behaviour of PPEK
Influence, be prepared for NA/TiO2/ PEEK trielement composite materials, and the friction and wear behavior of trielement composite material is examined
It examines.6.5 test NA/TiO2/ PEEK trielement composite material friction coefficient
Under different test conditions, friction coefficient (COF) such as the following table 2 of trielement composite material.
2 NA/TiO of table2The friction factor (COF) of/PEEK trielement composite materials
As shown in Table 2, under three kinds of different test conditions, 1%NA/3%TiO2The friction of/PEEK trielement composite materials
Factor is minimum, shows best wearability.Under the conditions of 2MPa, 200rpm, 1%NA/3%TiO2The friction of/PEEK because
Number is 0.1875,1%NA/5%TiO2The friction factor of/PEEK is 0.187, and the two remains basically stable, 2%NA/3%TiO2/PEEK
Friction factor be 0.2484, improve 32.5%, and after additional load or sliding speed double, 1%NA/3%
TiO2The wearability of/PEEK is still best, and friction factor is minimum, and with the NA/PEEK of identical adding proportion and TiO2/
The friction coefficient of PEEK composite materials reduces.If TiO2Content increases, then can be to NA/TiO2/ PEEK trielement composite materials are brought
Negative effect, friction factor increase, it can be seen that, in a certain range, nanometer diamond alkene (NA) and nano-titanium dioxide P25 are very
Synergistic effect is played well.
6.6 test NA/TiO2The wear rate of/PEEK trielement composite materials
Under different test conditions, wear rate such as the following table 3 of trielement composite material.
3 NA/TiO of table2The wear rate of/PEEK trielement composite materials
As shown in Table 3, under three kinds of different test conditions, 1%NA/3%TiO2The abrasion of/PEEK trielement composite materials
Rate is minimum, shows best wearability.Under the conditions of 2MPa, 200rpm, 1%NA/3%TiO2The wear rate of/PEEK is
1.2178×10-6mm3/ Nm, 1%NA/5%TiO2The wear rate of/PEEK is about 1.7630 × 10-6mm3/ Nm is improved
44.76%, 2%NA/3%TiO2The friction factor of/PEEK is 1.2868 × 10-6mm3/ Nm improves 5.7%.And attached
After load lotus or sliding speed double, 1%NA/3%TiO2The wearability of/PEEK is still best, and wear rate is minimum, and
With the NA/PEEK of identical adding proportion and TiO2The wear rate of/PEEK composite materials reduces.If TiO2Content raising then can
To NA/TiO2/ PEEK trielement composite materials are brought a negative impact, and wear rate increases.It can be seen that within the scope of certain proportion,
Nanometer diamond alkene (NA) and nano-titanium dioxide P25 have played synergistic effect well.
It can be seen that under more harsh environment, NA/TiO2/ PEEK trielement composite materials have better tribology
Performance improves the wearability of polyether-ether-ketone (PEEK), improves performance.The performance of this heterogeneous material is typically considered to
It is the stack result that each phase is contributed respectively, due to that during rubbing progress, some physics may occur between different phases, change
Act on, these significantly affect the friction and wear behavior of composite material.NA/TiO2/ PEEK trielement composite materials are rubbing
In the process, nano-titanium dioxide P25 is gathered in around nanometer diamond alkene, in friction process, in sample and steel disk between pair
Play the role of being fixed temporarily protection nanometer diamond alkene, prevents from being further damaged, nanometer diamond alkene is also made to be not easy from polyether-ether-ketone
(PEEK) it falls off in matrix, alleviates interfacial detachment degree, in addition, nano-titanium dioxide P25 may act as two mating surfaces
Between rolling element so that rolled to a certain extent between two mating surfaces rather than opposite sliding, and then reduce and cut
Shearing stress, friction factor and wear rate.
6.7 nano-titanium dioxide P25 are to TiO2The influence of the Vickers hardness of/PEEK composite materials
For polyether-ether-ketone base wear-resistant material, wearability is being influenced by material hardness size to a certain degree, such as material
Expecting that hardness is low may be such that wear rate increases, so the hardness for investigating modified composite material is necessary.Test nanometer two
Titanium oxide P25 is to TiO2The influence of the Vickers hardness of/PEEK composite materials, Vickers hardness figure (Vickers-hardness, HV)
As shown in Figure 5.
As shown in Figure 5, after filling nano-titanium dioxide P25, TiO2The hardness of/PEEK composite materials has certain amplitude
Ground improves, and nano-titanium dioxide P25 additive amounts are more, TiO2The hardness of/PEEK composite materials is higher.When without containing nanometer two
When titanium oxide P25, the Vickers hardness of pure polyetheretherketonematerials materials is about 22.5, when the content of nano-titanium dioxide P25 is 1%,
1%TiO2The Vickers hardness of/PEEK composite materials is 22.57, improves about 0.31%；When the content of nano-titanium dioxide P25
When being 3%, 3%TiO2The Vickers hardness of/PEEK composite materials is 22.94, improves about 1.95%；Work as nano-titanium dioxide
When the content of P25 is 5%, 5%TiO2The Vickers hardness of/PEEK composite materials is 23.58, improves about 4.8%；When nanometer two
When the content of titanium oxide P25 is 7%, 7%TiO2The Vickers hardness of/PEEK composite materials is 24.11, improves about 7.15%.
It can be seen that nano-titanium dioxide P25 can improve the hardness of polyether-ether-ketone (PEEK) material to a certain extent.
Influence of the 6.8 nanometer diamond alkene to the Vickers hardness of NA/PEEK composite materials
Test influence of the nanometer diamond alkene to the Vickers hardness of NA/PEEK composite materials, Vickers hardness figure (Vickers-
Hardness, HV) as shown in Figure 6.
It will be appreciated from fig. 6 that after filling nanometer diamond alkene, the hardness of NA/PEEK composite materials improves with having certain amplitude,
Nanometer diamond alkene additive amount is more, and the hardness of NA/PEEK composite materials is higher.Pure polyethers when without containing nanometer diamond alkene
The Vickers hardness of ether ketone material is about 22.5, when the content of nanometer diamond alkene is 1%, the Vickers of 1%NA/PEEK composite materials
Hardness is 24.6, improves about 9.3%；When the content of nanometer diamond alkene is 1.5%, the dimension of 1.5%NA/PEEK composite materials
Family name's hardness is 27.8, improves about 23.5%；When the content of nanometer diamond alkene is 2%, the dimension of 2%NA/PEEK composite materials
Family name's hardness is 32.6, improves about 44.8%；When the content of nanometer diamond alkene is 2.5%, 2.5%NA/PEEK composite materials
Vickers hardness be 40.2, improve about 78.6%；When the content of nanometer diamond alkene is 3%, 3%NA/PEEK composite materials
Vickers hardness be 50.8, improve about 125.7%, be free from 1.25 times of the hardness of nanometer diamond alkene.It can be seen that nanometer
The hardness of polyether-ether-ketone (PEEK) material can be significantly increased in diamond alkene.
6.9 test NA/TiO2The Vickers hardness of/PEEK trielement composite materials
The Vickers hardness of trielement composite material such as the following table 4.
4 NA/TiO of table2The Vickers hardness of/PEEK trielement composite materials
As shown in Table 4, NA/TiO2The more single nanometer diamond alkene of hardness or nanometer titanium dioxide of/PEEK trielement composite materials
Titanium P25 has for the hardness of the binary composite of additive significantly to be improved.1%NA/3%TiO2/ PEEK composite materials
Hardness is 25.6, and the hardness 22.5 of purer polyether-ether-ketone (PEEK) improves about 13.8%, compared with 1%NA/PEEK composite materials
Hardness 24.6 improves about 4.06%, compared with 3%TiO2/ PEEK composite hardnesses 22.94 improve about 11.6%；1%NA/
5%TiO2The hardness of/PEEK composite materials is 26.2, and the hardness 22.5 of purer polyether-ether-ketone (PEEK) improves about 16.4%,
Hardness 24.6 compared with 1%NA/PEEK composite materials improves about 7.3%, compared with 5%TiO2/ PEEK composite hardnesses 23.58 carry
It is high by about 11.1%；2%NA/3%TiO2The hardness of/PEEK composite materials is 33.8, the hardness of purer polyether-ether-ketone (PEEK)
22.5 improve about 50.2%, and the hardness 32.6 compared with 2%NA/PEEK composite materials improves about 3.7%, compared with 3%TiO2/PEEK
Composite hardness 22.94 improves about 47.3%.It follows that NA/TiO2The hardness of/PEEK trielement composite materials is purer poly-
Ether ether ketone (PEEK) and single nanometer diamond alkene or nano-titanium dioxide P25 be the hardness of the binary composite of additive all
Want high, nanometer diamond alkene and nano-titanium dioxide P25 play synergistic effect.
6.10NA/TiO2The thermal stability of/PEEK trielement composite materials
Since polyether-ether-ketone (PEEK) inherently has higher temperature classification, investigate the thermostabilization of composite material
Property, small table 5 is the 5% heat decomposition temperature T of weightlessness of each series material5%。
5 NA/TiO of table2The heat decomposition temperature of/PEEK trielement composite materials
As shown in Table 5, the thermal stability of pure polyether-ether-ketone (PEEK) is worst, heat decomposition temperature T5%It is 570 DEG C, 1%NA/
The heat decomposition temperature T of PEEK5%It is 588 DEG C, increases 18 DEG C, improves about 3.16%；3%TiO2The heat decomposition temperature of/PEEK
T5%It is 580 DEG C, increases 10 DEG C, improves about 1.75%；1%NA/3%TiO2The heat decomposition temperature T of/PEEK5%Highest is
598 DEG C, 28 DEG C are increased, improves about 4.9%, it can be seen that, the thermal stability of trielement composite material is greatly improved,
It can meet and be used under high temperature harsh environment.
The raising of the thermal stability of trielement composite material acts on the thermal consolidating of material from nano-particle, nano-particle
Addition, hinder to a certain extent polymer segment movement, simultaneously effective prevent the catabolite of most of polymer
Transport, therefore slow down thermal degradation process.
Claims (8)
1. a kind of polyether-ether-ketone composite material, which is characterized in that be made of the raw material of following weight percent：Polyether-ether-ketone 90~
96%, nanometer diamond alkene 1~3%, nano-titanium dioxide P25 1~7%.
2. polyether-ether-ketone composite material as described in claim 1, which is characterized in that the nanometer diamond alkene is by granularity
The nanometer diamond alkene of 50nm, 100nm, 200nm, 250nm form, the matter of the nanometer diamond alkene of 50nm, 100nm, 200nm, 250nm
Amount is than being (1 ~ 2) ︰ (2 ~ 3) ︰ (3 ~ 4) ︰ (4 ~ 5).
3. preparing the method that right will remove the polyether-ether-ketone composite material described in 1, which is characterized in that include the following steps：
1) it is according to mass ratio by nanometer diamond alkene, nano-titanium dioxide P25（1~3）︰（1~7）Ratio mixes, and obtains mixture
A；
2) in supersonic frequency is 40~60KHz, speed of agitator is under 30~60rpm, by deionized water and step 1) mixture A
It is stirred 25-35min, at 65-75 DEG C, then proceedes to that 3-aminopropyltriethoxysilane is added, reacts 3-4h, from
The heart, will centrifugation product drying, heat treatment, cooling modified mixture B, deionized water, three ethoxy of mixture A and 3- aminopropyl
The amount ratio of base silane is 100mL ︰ 1g ︰ 6mL；
3) by step 2) modified mixture B and polyether-ether-ketone mixing, melting extrusion, drying, injection molding, it is multiple to obtain polyether-ether-ketone
Condensation material.
4. the method as claimed in claim 3 for preparing polyether-ether-ketone composite material, which is characterized in that step 2）Centrifugal condition：
Centrifugal rotational speed is 4000~8000rpm, centrifugation time is 10~15min；Drying condition：Drying temperature is 60~80 DEG C, dries
Time is 4~12h.
5. the method as claimed in claim 4 for preparing polyether-ether-ketone composite material, which is characterized in that step 2）Middle heat treatment is adopted
It takes level Four staged to heat up, after first stage temperature rises to 60 DEG C by room temperature, keeps the temperature 30min；Second stage temperature is risen by 60 DEG C
To after 120 DEG C, 1h is kept the temperature；After phase III temperature rises to 280 DEG C by 120 DEG C, 3h is kept the temperature；Fourth stage temperature is risen by 280 DEG C
To after 400 DEG C, 10h is kept the temperature, during each step-up temperature, heating rate is 2~3 DEG C/min.
6. the method as claimed in claim 3 for preparing polyether-ether-ketone composite material, which is characterized in that step 3）Middle modified mixing
It when object B and polyether-ether-ketone mix, is placed in SHR high-speed mixers, is to be stirred under 42KW, speed of agitator 1050rpm in power of agitator
Mix 6~10min.
7. the method as claimed in claim 6 for preparing polyether-ether-ketone composite material, which is characterized in that step 3）Melting extrusion is adopted
Minipool rheometer is taken, processing temperature is 370 DEG C~395 DEG C, screw speed is 50~80rpm；Step 3）Drying condition：It is dry
Dry temperature is 120 DEG C, drying time 10h.
8. the method as claimed in claim 3 for preparing polyether-ether-ketone composite material, which is characterized in that step 1）Nanometer diamond
When alkene, nano-titanium dioxide P25 mixing, be placed in SHR high-speed mixers, in power of agitator be 42KW, speed of agitator 1050rpm
Under, stir 6~10min.
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