CN108517104B - Polyether-ether-ketone composite material and preparation method thereof - Google Patents
Polyether-ether-ketone composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyether-ether-ketone composite material which is prepared from the following raw materials in percentage by weight: 90-96% of polyether-ether-ketone, 1-3% of nano diamond alkene and 251-7% of nano titanium dioxide P. Also provides a corresponding preparation method. The nano diamond alkene and the nano titanium dioxide P25 play a synergistic role in reducing the friction factor and the wear rate in the composite material, the prepared ternary composite material is low in friction factor and wear rate, the wear of the material is reduced, the service life of the wear-resistant material is prolonged, the thermal stability is high, the ternary composite material can be used in a high-temperature harsh environment, and the application of PEEK is expanded.
Description
Technical Field
The invention belongs to the technical field of engineering materials, and particularly relates to a polyether-ether-ketone composite material and a preparation method thereof.
Background
In human social activities, the main causes of material failure are friction wear, fracture, corrosion and the like, and the friction wear causes 50% of material loss, namely, part of energy is wasted without being utilized. Furthermore, there are safety hazards to the frictional behaviour, for example, in mines, where frictional heating and sparks can cause fires, even explosions, causing accidents and losses; in the field of automobile parts, the damage of an engine, a shock absorber, a brake and the like is mainly caused by friction, and the automobile can be scrapped in the past; in the field of aerospace, the fuel is not tightly sealed or sparks are generated due to the reasons of corrosion resistance, friction and the like, so that the fuel is frequently exploded, and great financial loss is caused.
After entering the new century, with social progress and economic productivity development, friction materials are also urgently to be developed and applied, and various industries put forward higher requirements on friction-resistant materials, such as requirements on performances of enhanced wear resistance, corrosion resistance, wide application range, strong stability and the like. At present, the high polymer friction material gradually occupies the market due to excellent performance, and gradually replaces the friction equipment parts prepared by adopting metal materials.
Polyether ether ketone (PEEK) is a semi-crystalline thermoplastic special engineering plastic with excellent comprehensive performance, and is also the most widely and mainstream product in commercial polyaryletherketone, the main chain of the PEEK is composed of benzene rings, ether bonds and carbonyl groups, and the structural formula is shown in the specification.
The polyetheretherketone is used as a semicrystalline high temperature resistant resin, the maximum crystallinity is 48 percent, the crystallinity of a common product is 20 to 30 percent, and the glass transition temperature T isgIs 143 ℃ and a melting point TmIs 343 ℃, which has mainly the following excellent properties:
1. the heat resistance is good, the long-term use temperature can reach 250 ℃, the short-time work can be realized even at the temperature of 300 ℃, and the heat resistance is far higher than that of polycarbonate, ABS and other resins;
2. the mechanical property is good, the polyether-ether-ketone has extremely high modulus and strength, can be compared favorably with thermosetting materials, simultaneously has good toughness, impact resistance and fatigue resistance, has good comprehensive performance, and is beneficial to prolonging the service life of parts;
3. the product has good dimensional stability and small thermal expansion coefficient;
4. the wear resistance is good, and the polyether-ether-ketone has self-lubricating property and lower friction coefficient and wear loss;
5. the flame retardant property is good, and the polyether-ether-ketone has self-extinguishing property and meets strict safety requirements;
6. the corrosion resistance is excellent, the chemical property of the polyether-ether-ketone is stable, the polyether-ether-ketone is hardly dissolved in any other acid-base or organic reagent except concentrated sulfuric acid, and the corrosion resistance is excellent;
7. the insulating material has the advantages that the insulating material is electrically insulating, the dielectric constant of the insulating material is 3.2-3.3, the dielectric loss is 0.0016 under 1KHz, the breakdown voltage is 17KV/mm, the arc resistance is 175V, the insulating material can be used as a C-grade insulating material, and meanwhile, the insulating material is stable in electrical insulating performance and does not change along with the changes of temperature, humidity and current frequency;
8. the polyether-ether-ketone resin has excellent processability, is thermoplastic resin, can be subjected to secondary processing, has good fluidity, is easy to extrude and injection mold, and has high molding efficiency.
Therefore, the method is widely applied to the fields of spaceflight, military, industry, energy sources and the like.
However, at present, the requirement for the friction-resistant material is higher and higher, so that the material can still be normally used in a harsh working environment, for example, under conditions of high load, high sliding speed and high temperature, the material must also maintain low friction coefficient and abrasion loss, and the polyetheretherketone resin cannot meet the use requirement of harsh work change, so that the polyetheretherketone resin needs to be modified to reduce the friction coefficient and abrasion loss and widen the application range of the polyetheretherketone.
Disclosure of Invention
The invention aims to provide a polyetheretherketone composite material, and simultaneously provides a corresponding preparation method thereof, which is another invention aim of the invention.
Based on the purpose, the invention adopts the following technical scheme:
a polyether-ether-ketone composite material is prepared from the following raw materials in percentage by weight: 90-96% of polyether-ether-ketone, 1-3% of nano diamond alkene and 251-7% of nano titanium dioxide P.
The nano-diamond alkene consists of nano-diamond alkene with the granularity of 50nm, 100nm, 200nm and 250nm, and the mass ratio of the nano-diamond alkene with the granularity of 50nm, 100nm, 200nm and 250nm is (1-2): 2-3): 3-4): 4-5.
A method of preparing a polyetheretherketone composite comprising the steps of:
1) mixing nano diamond alkene and nano titanium dioxide P25 according to the mass ratio of (1-3): 1-7 to obtain a mixture A;
2) stirring and mixing deionized water and the mixture A obtained in the step 1) for 25-35min at an ultrasonic frequency of 40-60 KHz and a stirring rotation speed of 30-60 rpm, then continuously adding 3-aminopropyltriethoxysilane at 65-75 ℃, reacting for 3-4h, centrifuging, drying a centrifugal product, performing heat treatment, and cooling to obtain a modified mixture B, wherein the dosage ratio of the deionized water to the mixture A to the 3-aminopropyltriethoxysilane is 100 mL: 1 g: 6 mL;
3) and (3) mixing the modified mixture B obtained in the step 2) with the polyether-ether-ketone, performing melt extrusion, drying, and performing injection molding to obtain the polyether-ether-ketone composite material.
Step 2) centrifugation conditions: the centrifugal speed is 4000-8000 rpm, and the centrifugal time is 10-15 min; drying conditions are as follows: the drying temperature is 60-80 ℃, and the drying time is 4-12 h.
Step 2), four-stage stepwise heating is adopted for heat treatment, and the temperature in the first stage is raised from normal temperature to 60 ℃, and then is kept for 30 min; in the second stage, the temperature is increased from 60 ℃ to 120 ℃, and then the temperature is kept for 1 h; in the third stage, the temperature is increased from 120 ℃ to 280 ℃, and then the temperature is kept for 3 hours; and (3) after the temperature of the fourth stage is increased from 280 ℃ to 400 ℃, preserving the heat for 10 hours, wherein the heating rate is 2-3 ℃/min in the heating process of each stage.
And 3) when the modified mixture B in the step 3) is mixed with the polyether-ether-ketone, placing the mixture in an SHR high-speed mixer, and stirring for 6-10 min at a stirring power of 42KW and a stirring rotation speed of 1050 rpm.
Step 3), adopting a micro-mixing rheometer for melt extrusion, wherein the processing temperature is 370-395 ℃, and the screw rotation speed is 50-80 rpm; step 3) drying conditions: the drying temperature is 120 ℃, and the drying time is 10 h.
And step 1), when mixing the nano diamond alkene and the nano titanium dioxide P25, placing the mixture into an SHR high-speed mixer, and stirring for 6-10 min at a stirring power of 42KW and a stirring rotation speed of 1050 rpm.
Compared with the prior art, the invention has the following beneficial effects:
the invention has the advantages that:
1. the nano diamond alkene and the nano titanium dioxide P25 are added into the ternary composite material, the nano diamond alkene has no toxic or side effect on human bodies, the nano diamond alkene is high in hardness, strong in wear resistance and high in stability, the friction factor and the wear rate of the composite material can be reduced, the nano diamond alkene and the nano titanium dioxide P25 play a synergistic effect in reducing the friction factor and the wear rate in the composite material, the prepared ternary composite material is low in friction factor and wear rate, the wear of the material is reduced, the service life of the wear-resistant material is prolonged, the thermal stability is high, the requirement of using the composite material in a high-temperature harsh environment can be met, and the application of PEEK is expanded;
2. the preparation method is simple, easy to operate, less in used equipment and low in production cost.
Drawings
FIG. 1 shows the addition amount of different nano-titanium dioxide P25 to TiO2The friction coefficient effect of the/PEEK composite;
FIG. 2 shows the amount of different nano-titanium dioxide P25 added to TiO2Wear rate impact of/PEEK composite;
FIG. 3 shows the effect of different amounts of nanodiamond-limonene added on the friction factor of NA/PEEK composite materials;
FIG. 4 is a graph of the effect of different nanodiamond alkene additions on the wear rate of NA/PEEK composites;
FIG. 5 shows the nano-titanium dioxide P25 vs. TiO2Effect of vickers hardness of the/PEEK composite;
FIG. 6 is a graph showing the effect of nanodiamond-limonene on Vickers hardness of NA/PEEK composites.
Detailed Description
Example 1
A polyether-ether-ketone composite material is prepared from the following raw materials in percentage by weight: 96% of polyether-ether-ketone, 1% of nano diamond alkene and 253% of nano titanium dioxide.
The nano-diamond alkene comprises nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm, and the mass ratio of the nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm is 1: 2: 3: 4.
A method of preparing a polyetheretherketone composite comprising the steps of:
1) placing nano diamond alkene and nano titanium dioxide P25 in an SHR high-speed mixer according to a mass ratio of 1: 3, and stirring for 10min at a stirring power of 42KW and a stirring rotation speed of 1050rpm to obtain a mixture A;
2) stirring and mixing 100mL of deionized water and 1g of the mixture A obtained in the step 1) for 30min at the ultrasonic frequency of 40KHz and the stirring speed of 30rpm, continuously stirring, dropwise adding 6mL of 3-aminopropyltriethoxysilane, reacting for 4h at the reaction temperature of 70 ℃, centrifuging for 15min at the centrifugal speed of 4000rpm, drying the centrifuged product (mainly nano diamond alkene and nano titanium dioxide P25) for 12h at the temperature of 60 ℃, performing high-temperature heat treatment, and naturally cooling to obtain a modified mixture B; the high-temperature heat treatment adopts four-stage stepwise temperature rise, and the temperature is raised from normal temperature to 60 ℃ in the first stage and then is kept for 30 min; in the second stage, the temperature is increased from 60 ℃ to 120 ℃, and then the temperature is kept for 1 h; in the third stage, the temperature is increased from 120 ℃ to 280 ℃, and then the temperature is kept for 3 hours; after the temperature of the fourth stage is increased from 280 ℃ to 400 ℃, the heat is preserved for 10h, the temperature rising rate is 2 ℃/min in the temperature rising process of each stage,
3) placing the modified mixture B and the polyether-ether-ketone obtained in the step 2) into an SHR high-speed mixer, stirring for 10min at a stirring power of 42KW and a stirring rotation speed of 1050rpm, at a processing temperature of 395 ℃ and a screw rotation speed of 50rpm, performing melt extrusion by using a micro-mixing rheometer (HAAKE MiniLab, Sammer Feishel technology, wherein the screw rotates in a conical direction), placing into a 120 ℃ oven, drying for 10h, and performing injection molding by using a micro-injection molding machine (HAAKE MiniJet, Sammer Feishel technology) under the conditions that: the temperature of the charging barrel is 395 ℃, the temperature of the die cavity is 180 ℃, the injection pressure is 900bar, the holding time is 20s, the holding pressure is 700bar, the holding time is 20s, the constant temperature heat treatment is carried out for 2h at the temperature of 200 ℃, and the annealing is carried out to the normal temperature, so as to obtain the polyether-ether-ketone composite material.
Example 2
A polyether-ether-ketone composite material is prepared from the following raw materials in percentage by weight: 94% of polyether-ether-ketone, 1% of nano diamond alkene and 255% of nano titanium dioxide P.
The nano-diamond alkene comprises nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm, and the mass ratio of the nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm is 1: 2: 3: 4.
Method for preparing a polyetheretherketone composite reference is made to example 1.
Example 3
A polyether-ether-ketone composite material is prepared from the following raw materials in percentage by weight: 95% of polyether-ether-ketone, 2% of nano diamond alkene and 253% of nano titanium dioxide.
The nano-diamond alkene comprises nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm, and the mass ratio of the nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm is 1: 2: 3: 4.
Method for preparing a polyetheretherketone composite reference is made to example 1.
Example 4
A polyether-ether-ketone composite material is prepared from the following raw materials in percentage by weight: 90% of polyether-ether-ketone, 3% of nano diamond alkene and 257% of nano titanium dioxide P.
The nano-diamond alkene comprises nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm, and the mass ratio of the nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm is 2: 3: 4: 5.
A method of preparing a polyetheretherketone composite comprising the steps of:
1) placing nano diamond alkene and nano titanium dioxide P25 in an SHR high-speed mixer according to a mass ratio of 3: 7, and stirring for 6min at a stirring power of 42KW and a stirring rotation speed of 1050rpm to obtain a mixture A;
2) stirring and mixing 100mL of deionized water and 1g of the mixture A obtained in the step 1) for 30min at an ultrasonic frequency of 60KHz and a stirring speed of 60rpm, continuously stirring, dropwise adding 6mL of 3-aminopropyltriethoxysilane into the mixture A dropwise, reacting for 4h at a reaction temperature of 70 ℃, centrifuging for 10min at a centrifugal speed of 8000rpm, drying the centrifuged products (mainly nano-diamond alkene and nano-titanium dioxide P25) for 4h at a drying temperature of 60 ℃, and performing high-temperature heat treatment and natural cooling to obtain a modified mixture B; the high-temperature heat treatment adopts four-stage stepwise temperature rise, and the temperature is raised from normal temperature to 60 ℃ in the first stage and then is kept for 30 min; in the second stage, the temperature is increased from 60 ℃ to 120 ℃, and then the temperature is kept for 1 h; in the third stage, the temperature is increased from 120 ℃ to 280 ℃, and then the temperature is kept for 3 hours; after the temperature of the fourth stage is increased from 280 ℃ to 400 ℃, the heat is preserved for 10h, the temperature rising rate is 3 ℃/min in the temperature rising process of each stage,
3) placing the modified mixture B and the polyether-ether-ketone obtained in the step 2) into an SHR high-speed mixer, stirring for 6min at a stirring power of 42KW and a stirring rotation speed of 1050rpm, at a processing temperature of 370 ℃ and a screw rotation speed of 50rpm, performing melt extrusion by using a micro-mixing rheometer (HAAKE MiniLab, Sammer Feishel technology, wherein the screw rotates in a conical direction), placing into a 120 ℃ oven, drying for 10h, and performing injection molding by using a micro-injection molding machine (HAAKE MiniJet, Sammer Feishel technology) under the conditions that: the temperature of the charging barrel is 380 ℃, the temperature of the die cavity is 180 ℃, the injection pressure is 900bar, the holding time is 20s, the holding pressure is 700bar, the holding time is 20s, the constant temperature heat treatment is carried out for 2h at the temperature of 200 ℃, and the annealing is carried out to the normal temperature, so as to obtain the polyether-ether-ketone composite material.
Example 5
A polyether-ether-ketone composite material is prepared from the following raw materials in percentage by weight: 92% of polyether-ether-ketone, 2% of nano diamond alkene and 256% of nano titanium dioxide P.
The nano-diamond alkene comprises nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm, and the mass ratio of the nano-diamond alkene with the particle size of 50nm, 100nm, 200nm and 250nm is 2: 3: 4: 5.
Method for preparing a polyetheretherketone composite reference is made to example 4.
Example 6 Performance testing
Hardness testing of composite materials
The composite material sample after injection molding is utilized, the surface is smooth and flat, the composite material sample is cylindrical, the diameter is 15mm, the height is 1.5mm, an electronic digital display Vickers hardness tester (MHV-30Z) is adopted for hardness testing, and the testing conditions are as follows: load 2Kg, hold pressure 15s, and test ten sets of replicates for each sample, and take the average.
Tribological behavior characterization of composite materials
A sample of the composite material after injection moulding, cylindrical, 6.3mm in diameter and 18.8mm in height, was subjected to a multifunctional friction tester (UMT-2, Bruker, Germany) according to ASTM G99-04, pin-disk contact type, one-way sliding, friction couple 45#Stainless steel (diameter 50mm, height 10mm), with different roughness (900) before each test#And 1500#) The water sand paper is used for grinding and polishing the surface of a sample and the surface of a friction pair steel disc, then the sample and the steel disc which are subjected to ultrasonic cleaning and grinding and polishing are cleaned by acetone, dried and cooled, and the initial weight m is weighed by an electronic digital display balance1After the tribology test is finished, the sample is ultrasonically cleaned by acetone again, dried and cooled, and the weight m of the sample after the test is weighed2. In order to examine the tribological behavior of the composite material under different loads and sliding speeds, the test conditions were 2MPa (62.32N), 200rpm (0.42m/s), respectively; 2MPa (62.32N), 400rpm (0.84 m/s); 4MPa (124.64N), 200rpm (0.42 m/s). The test time for each sample was 2h, and at least three replicates of each group were averaged.
The change curve of the friction factor of the composite material along with time is recorded by software of an instrument, and the formula of the wear rate is as follows:
wherein: volumetric wear rate (mm) of Ws-composite3/N·m)，m1Mass (g), m of the sample before the rub test2Mass of sample after rub test (g), p-density of sample (g/cm)3) F-friction test applied load (N), L-friction test total sliding distance (m),
the density ρ was measured by the principle of drainage method using an electronic digital display densitometer (Mettler SD-200L).
Thermal stability of composite materials
Investigating the thermal stability of the composite material by using a thermogravimetric analyzer (Pyris 1 TGA, Perkin Elmer), taking 3-5 mg of dried extruded granules, keeping the temperature at 100 ℃ for 10min under the test atmosphere of nitrogen, heating to 800 ℃ at the heating rate of 10 ℃/min, and calculating the thermal decomposition temperature T with 5% weight loss according to the obtained thermal weight loss curve5％。
The composition of each set of test samples is shown in table 1 below (page 7 of raw material), and NA is nanodiamond.
TABLE 1 composition of test samples
| 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 optimal filling amount of nano-diamond alkene and nano-titanium dioxide P25 in a polyether-ether-ketone matrix, firstly, the frictional wear behavior of the PEEK composite material singly filled and modified by nano-diamond alkene and nano-titanium dioxide P25 is considered, the influence of different filling amounts on the frictional wear performance of the PEEK composite material (the preparation method is referred to as example 1) is considered, and meanwhile, the change conditions of the frictional factor and the wear rate of the PEEK composite material under different frictional environments (different loads and different sliding speeds) are considered.
6.1 addition of different amounts of Nano-Titania P25 to TiO2Effect of the Friction-wear Properties of the PEEK composite
As shown in fig. 1, test conditions, a: 2MPa, 200rpm and 2 h; b: 2MPa, 400rpm and 2 h; c: 4MPa, 200rpm, 2 h.
As can be seen from FIG. 1, under different test conditions, when the content of the nano titanium dioxide P25 is in the range of 1% -7%, TiO was added2The friction factor of the PEEK composite material shows the tendency of firstly decreasing and then increasing, and 3 percent of TiO2the/PEEK composite material shows the best tribological behaviour with the lowest friction factor. Under the conditions of 2MPa and 200rpm, the friction factor of the pure PEEK material without the nano titanium dioxide P25 is about 0.433, the friction factor is gradually reduced along with the increase of the addition amount of the nano titanium dioxide P25, and when the addition amount of the nano titanium dioxide P25 is 1%, 1% of TiO is added2The friction factor of the/PEEK composite material is about 0.422, which is reduced by about 2.54%; when the addition amount of the nano titanium dioxide P25 is 3 percent, 3 percent of TiO2The friction factor of the/PEEK composite material is the lowest, about 0.4057, which is reduced by about 6.3%; when the addition amount of the nano titanium dioxide P25 is 5 percent, 5 percent of TiO2The friction factor of the/PEEK composite material rises to about 0.424, which is reduced by about 2.07%; when the addition amount of the nano titanium dioxide P25 is 7 percent, 7 percent of TiO2PEEK composite materialThe friction factor of the material rose to about 0.43, which is substantially the same as that of pure PEEK without the addition of nano-titania P25.
When the load or sliding speed increases, the TiO2The friction factor of the/PEEK composite material also shows a tendency to decrease first and then increase. In TiO2In the PEEK system, TiO2After the friction additional load or the sliding speed of the PEEK composite material is doubled, the friction factors are increased, and 3 percent of TiO is used2The PEEK is taken as an example, and the friction factor is about 0.432 at 4MPa and about 6.5% rise at the same rotation speed, and about 0.43 at 400rpm and about 6% rise at the same load.
6.2 addition of different amounts of Nano-Titania P25 to TiO2Effect of wear Rate of/PEEK composites
As shown in fig. 2, test conditions, a: 2MPa, 200rpm and 2 h; b: 2MPa, 400rpm and 2 h; c: 4MPa, 200rpm, 2 h.
As can be seen from FIG. 2, under different test conditions, when the content of the nano titanium dioxide P25 is in the range of 1% -7%, TiO was added2The wear rate of the PEEK composite material shows a trend of decreasing and then increasing, and 3 percent of TiO2The wear rate of the/PEEK composite is lowest. The wear rate of the pure PEEK material without the nano titanium dioxide P25 is about 4.48mm under 2MPa and 200rpm3N.m, the wear rate is gradually reduced along with the increase of the addition amount of the nano titanium dioxide P25, and when the addition amount of the nano titanium dioxide P25 is 1 percent, 1 percent of TiO2The wear rate of the PEEK composite material is about 3.8mm3A reduction of about 13.6% in/N.m; when the addition amount of the nano titanium dioxide P25 is 3 percent, 3 percent of TiO2The wear rate of the/PEEK composite material is the lowest and is about 3.4mm3A reduction of about 22.7% in/N.m; when the addition amount of the nano titanium dioxide P25 is 5 percent, 5 percent of TiO2The wear rate of the/PEEK composite material is increased to about 3.6mm3A reduction of about 18.18% in/N.m; when the addition amount of the nano titanium dioxide P25 is 7 percent, 7 percent of TiO2The wear rate of the/PEEK composite material is increased to about 5.5mm3The abrasion rate of the PEEK is higher than that of pure PEEK without the nano titanium dioxide P25, and is improved by about 25 percent.
When the load or sliding speed increases, the TiO2The wear rate of the/PEEK composite also shows a tendency to decrease first and then increase. In TiO2In the PEEK system, TiO2After the friction additional load or the sliding speed of the PEEK composite material is doubled, the wear rate is increased, and 3 percent of TiO is used2The PEEK is used as an example to illustrate that the wear rate is about 5.25mm under the condition of 4MPa at the same rotating speed3N.m, increased by about 53.2%, and a wear rate of about 5.74mm at 400rpm under the same load3The increase in/N.m was about 67.6%.
6.3 Effect of different amounts of Nano Diamond alkene on the Friction factor of NA/PEEK composite Material
As shown in fig. 3, test conditions, a: 2MPa, 200rpm and 2 h; b: 2MPa, 400rpm and 2 h; c: 4MPa, 200rpm, 2 h.
As shown in FIG. 3, under different test conditions, when the content of nanodiamond-ene is in the range of 1% to 3%, the friction factor of the NA/PEEK composite material shows a tendency of rapidly decreasing first and then slowly increasing, and when the filling amount of nanodiamond-ene is in the range of 1% to 2%, the composite material shows the best tribology behavior, and the friction factor is the lowest. Under the conditions of 2MPa and 200rpm, the friction factor of the pure PEEK material without the nano diamond alkene is about 0.433, and when the addition amount of the nano diamond alkene is 1%, the friction factor of the 1% NA/PEEK composite material is about 0.21, and the friction factor is rapidly reduced by about 51.5%; when the addition amount of the nano diamond alkene is 1-2%, the friction factor of the NA/PEEK composite material is kept stable and kept at 0.21-0.22; when the addition amount of the nano diamond alkene is 2.5%, the friction factor of the 2.5% NA/PEEK composite material is increased to about 0.25, and is reduced by about 42.2%; when the addition amount of the nano diamond alkene is 3%, the friction factor of the 3% NA/PEEK composite material continues to rise to about 0.28, and is reduced by about 35.3%.
When the load or sliding speed is increased, the friction factor of the NA/PEEK composite material also shows a tendency of first decreasing rapidly and then increasing slowly. In the NA/PEEK system, after the friction additional load or the sliding speed of the NA/PEEK composite material is doubled, the friction factor is reduced, and by taking 1% of NA/PEEK as an example, the friction factor is about 0.14 and is reduced by about 67.6% under the condition of 4MPa at the same rotating speed, and the friction factor is about 0.18 and is reduced by about 58.4% under the condition of 400rpm at the same load.
6.4 Effect of different amounts of Nano Diamond alkene on the wear Rate of NA/PEEK composite Material
As shown in fig. 4, test conditions, a: 2MPa, 200rpm and 2 h; b: 2MPa, 400rpm and 2 h; c: 4MPa, 200rpm, 2 h.
As shown in FIG. 4, under different test conditions, when the content of nanodiamond-ene is in the range of 1% to 3%, the wear rate of the NA/PEEK composite material tends to decrease rapidly and increase slowly, and when the addition amount of nanodiamond-ene is in the range of 1% to 2%, the wear rate of the NA/PEEK composite material is the lowest and stable. Under the conditions of 2MPa and 200rpm, the wear rate of the pure PEEK material without the nano diamond alkene is about 4.48mm3N.m, the wear rate decreases rapidly with increasing nano diamond alkene, and when the nano diamond alkene is added to 1%, the wear rate of 1% NA/PEEK composite material is about 1.46mm3A reduction of about 67.4% in/N.m; when the addition amount of the nano diamond alkene is 1.5 percent, the wear rate of the 1.5 percent NA/PEEK composite material is about 1.48mm3A reduction of about 66.9% in/N.m; when the addition amount of the nano diamond alkene is 2 percent, the wear rate of the 2 percent NA/PEEK composite material is about 1.5mm3The reduction in/N.m is about 66.5%. It can be seen that when the amount of nanodiamond-ene added is in the range of 1% to 2%, the wear rate of the NA/PEEK composite material is low and stable, and when the amount of nanodiamond-ene added is 2.5%, the wear rate of the 2.5% NA/PEEK composite material is increased to about 2.2mm3the/N.m is reduced by about 50.9%, when the addition amount of the nano diamond alkene is 3%, the wear rate of the 2.5% NA/PEEK composite material is continuously increased to about 2.3mm3The reduction in/N.m is about 48.6%.
The wear rate of the NA/PEEK composite also shows a tendency to decrease and then increase as the load or sliding speed increases. In the NA/PEEK system, after the friction additional load or the sliding speed of the NA/PEEK composite material is doubled, the wear rate is increased, which is illustrated by taking 1% of NA/PEEK as an example, and the NA/PEEK composite material is ground under the condition of 4MPa at the same rotating speedThe damage rate is about 1.8mm3N.m, increased by about 23.3%, and a wear rate of about 1.7mm at 400rpm under the same load3The increase in/N.m is about 16.4%.
The friction factor of the composite material is mainly influenced by factors such as real friction contact area, material shear strength, material surface energy and the like,
wherein mu is a friction factor, F is a friction force, A is a real friction contact area, P is an additional load, and tau is the shearing strength of the material. When the additional load or the sliding speed is increased, on one hand, the real friction contact area is increased, the friction heat is increased, the friction surface is softened, the elastic deformation and the plastic deformation are increased, so that the friction factor is increased, and on the other hand, the softening and the micro-flowing of the friction surface of the material can reduce the shearing strength of the material, so that the friction factor is reduced. For the nano diamond alkene additive, the load is increased or the sliding speed is increased to be equivalent to the severity of increasing the friction condition, the friction and the grinding of the friction dual-face steel disc on the surface of the material are intensified, the nano diamond alkene falls off along with the friction of the PPEK, so that more nano diamond alkene is exposed, and the nano diamond alkene is of a layered structure, so that a more complete and uniform friction transfer film is formed, a better lubricating effect is achieved, and the friction factor is reduced. For the nano titanium dioxide P25 additive, when the addition amount of the nano titanium dioxide P25 is low, one side of nano titanium dioxide P25 particles can support load, and on the other hand, the nano titanium dioxide P25 particles fall off along with friction and fill gaps between microscopic unevenness in friction fit to serve as balls, so that the real friction area is reduced, the friction factor is reduced, when the addition amount of the nano titanium dioxide P25 is high, the nano titanium dioxide P25 particles fall off along with friction, the nano titanium dioxide P25 particles are agglomerated due to large specific surface energy, large-particle abrasive particles are formed, the abrasion to the surface is accelerated, and the friction factor and the abrasion rate are increased.
The influence of the nano titanium dioxide P25 and the nano diamond alkene as single fillers on the friction performance of the PPEK is researched to prepare the NA/TiO2The PEEK ternary composite material is subjected to frictional wear actionThe investigation was carried out. 6.5 testing of NA/TiO2Friction coefficient of PEEK ternary composite material
The coefficient of friction (COF) of the ternary composites under the different test conditions is shown in table 2 below.
TABLE 2 NA/TiO2Friction factor (COF) of PEEK ternary composite material
As can be seen from Table 2, 1% NA/3% TiO under three different test conditions2The PEEK ternary composite material has the lowest friction factor and shows the best wear resistance. 1% NA/3% TiO at 2MPa, 200rpm2PEEK has a friction factor of 0.1875, 1% NA/5% TiO2The friction factor of the/PEEK was 0.187, which is essentially equal, 2% NA/3% TiO2The friction factor of the/PEEK was 0.2484, an improvement of 32.5%, and after doubling the additional load or the sliding speed, 1% NA/3% TiO2The wear resistance of the/PEEK is still the best, the friction factor is the lowest, and the same adding proportion of NA/PEEK and TiO is added2The friction coefficient of the PEEK composite material is reduced. If TiO2When the content is increased, the content will be increased to NA/TiO2The PEEK ternary composite material has negative effects and the friction factor is increased, so that the nano diamond alkene (NA) and the nano titanium dioxide P25 well exert a synergistic effect in a certain range.
6.6 testing of NA/TiO2Wear rate of/PEEK ternary composite material
The wear rates of the ternary composites under the different test conditions are shown in table 3 below.
TABLE 3 NA/TiO2Wear rate of/PEEK ternary composite material
As can be seen from Table 3, 1% NA/3% TiO under three different test conditions2The wear rate of the/PEEK ternary composite material is lowest, and the best wear resistance is shown. Under the conditions of 2MPa and 200rpm, 1% NA/3% TiO2The wear rate of the PEEK is 1.2178X 10-6mm3/N·m，1％NA/5％TiO2The wear rate of PEEK is about 1.7630X 10-6mm3Increased by 44.76% for N.m, 2% NA/3% TiO2PEEK having a Friction factor of 1.2868X 10-6mm3The ratio of the carbon atoms to the carbon atoms is increased by 5.7 percent. And 1% NA/3% TiO after doubling the additional load or glide speed2The wear resistance of the/PEEK is still the best, the wear rate is the lowest, and the same adding proportion of NA/PEEK and TiO is added2The wear rate of the/PEEK composite material is reduced. If TiO2The content of the catalyst is increased to NA/TiO2The PEEK ternary composite material has negative effects and the wear rate is increased. Therefore, the nano diamond alkene (NA) and the nano titanium dioxide P25 well exert a synergistic effect in a certain proportion range.
It can be seen that in more severe environments, NA/TiO2The PEEK ternary composite material has better tribological performance, improves the wear resistance of the PEEK and improves the performance. The performance behavior of such multiphase materials is generally considered to be a superposition of the individual contributions of the phases, since during the course of the friction, some physical, chemical interactions may occur between the different phases, which greatly influence the tribological wear behavior of the composite material. NA/TiO2In the friction process of the/PEEK ternary composite material, the nano titanium dioxide P25 gathers around the nano diamond alkene, the effect of temporarily fixing and protecting the nano diamond alkene is achieved between a sample and a steel disc matching pair in the friction process, further damage is prevented, the nano diamond alkene is not prone to falling off from a polyether ether ketone (PEEK) matrix, the interface debonding degree is reduced, in addition, the nano titanium dioxide P25 can serve as a rolling body between two matching surfaces, the two matching surfaces roll to a certain degree instead of relative sliding, and then the shearing stress, the friction factor and the wear rate are reduced.
6.7 nanometer titanium dioxide P25 vs. TiO2Influence of Vickers hardness of the/PEEK composite
In the case of the polyether ether ketone based wear-resistant material, the wear resistance is influenced to a certain extent by the hardness of the material, for example, the wear rate may be increased due to the low hardness of the material, so that it is necessary to examine the hardness of the modified composite material. Testing of Nano-Titania P25 vs. TiO2The effect of Vickers hardness of the/PEEK composite is shown in FIG. 5, the Vickers-hardness, HV diagram.
As can be seen from FIG. 5, after filling with nano-titanium dioxide P25, TiO was added2The hardness of the PEEK composite material is improved to a certain extent, and the more the nano titanium dioxide P25 is added, the more TiO is added2The higher the stiffness of the/PEEK composite. When the nano titanium dioxide P25 is not contained, the Vickers hardness of the pure polyetheretherketone material is about 22.5, and when the content of the nano titanium dioxide P25 is 1%, the 1% TiO is2The Vickers hardness of the/PEEK composite material is 22.57, which is improved by about 0.31 percent; when the content of the nano titanium dioxide P25 is 3 percent, 3 percent of TiO2The Vickers hardness of the/PEEK composite material is 22.94, which is improved by about 1.95 percent; when the content of the nano titanium dioxide P25 is 5 percent, 5 percent of TiO2The Vickers hardness of the/PEEK composite material is 23.58, which is improved by about 4.8 percent; when the content of the nano titanium dioxide P25 is 7 percent, 7 percent of TiO2The Vickers hardness of the/PEEK composite material is 24.11, which is improved by about 7.15%. Therefore, the nano titanium dioxide P25 can improve the hardness of the Polyetheretherketone (PEEK) material to a certain extent.
6.8 Effect of nanodiamond-limonene on Vickers hardness of NA/PEEK composite
The effect of nanodiamond olefins on the Vickers hardness of NA/PEEK composites was tested and the Vickers-hardness plot (HV) is shown in fig. 6.
As can be seen from FIG. 6, the hardness of the NA/PEEK composite material was improved to a certain extent after the nano-diamond alkene was filled, and the hardness of the NA/PEEK composite material was increased as the amount of nano-diamond alkene added was increased. When the pure polyetheretherketone material does not contain nano diamond alkene, the Vickers hardness of the pure polyetheretherketone material is about 22.5, and when the content of the nano diamond alkene is 1%, the Vickers hardness of the 1% NA/PEEK composite material is 24.6, which is improved by about 9.3%; when the content of the nano diamond alkene is 1.5 percent, the Vickers hardness of the 1.5 percent NA/PEEK composite material is 27.8, which is improved by about 23.5 percent; when the content of the nano diamond alkene is 2%, the Vickers hardness of the 2% NA/PEEK composite material is 32.6, which is improved by about 44.8%; when the content of the nano diamond alkene is 2.5 percent, the Vickers hardness of the 2.5 percent NA/PEEK composite material is 40.2, which is improved by about 78.6 percent; when the nanodiamond-ene content was 3%, the vickers hardness of the 3% NA/PEEK composite was 50.8, which increased by about 125.7%, which was 1.25 times the hardness without nanodiamond-ene. Therefore, the nano diamond alkene can greatly improve the hardness of the Polyetheretherketone (PEEK) material.
6.9 testing of NA/TiO2Vickers hardness of/PEEK ternary composite material
The vickers hardness of the ternary composite is shown in table 4 below.
TABLE 4 NA/TiO2Vickers hardness of/PEEK ternary composite material
As can be seen from Table 4, NA/TiO2Compared with the binary composite material taking single nanometer diamond alkene or nanometer titanium dioxide P25 as an additive, the hardness of the/PEEK ternary composite material is obviously improved. 1% NA/3% TiO2The hardness of the/PEEK composite material is 25.6, which is improved by about 13.8% compared with the hardness of pure Polyetheretherketone (PEEK) of 22.5, about 4.06% compared with the hardness of 1% NA/PEEK composite material of 24.6, and about 3% TiO2The hardness of the PEEK composite material is improved by about 11.6 percent; 1% NA/5% TiO2The hardness of the/PEEK composite material is 26.2, which is improved by about 16.4% compared with the hardness of pure Polyetheretherketone (PEEK) of 22.5, about 7.3% compared with the hardness of 1% NA/PEEK composite material of 24.6, and about 5% TiO2The hardness of the PEEK composite material is improved by about 11.1 percent; 2% NA/3% TiO2The hardness of the/PEEK composite material is 33.8, which is improved by about 50.2% compared with the hardness of pure Polyetheretherketone (PEEK) of 22.5, improved by about 3.7% compared with the hardness of 2% NA/PEEK composite material of 32.6, and improved by 3% TiO2PEEK composite materialThe material hardness is improved by about 47.3 percent by 22.94 percent. Thus, it was found that NA/TiO2The hardness of the PEEK ternary composite material is higher than that of a binary composite material taking pure Polyetheretherketone (PEEK) and single nano-diamond alkene or nano-titanium dioxide P25 as additives, and the nano-diamond alkene and the nano-titanium dioxide P25 play a synergistic role.
6.10NA/TiO2Thermal stability of/PEEK ternary composite material
Since Polyetheretherketone (PEEK) itself has a high heat resistance rating, the thermal stability of the composite material was examined and the small Table 5 shows the weight loss 5% thermal decomposition temperature T of each series of materials5％。
TABLE 5 NA/TiO2Thermal decomposition temperature of PEEK ternary composite material
As can be seen from Table 5, pure Polyetheretherketone (PEEK) has the worst thermal stability and a thermal decomposition temperature T5％At 570 ℃ and a thermal decomposition temperature T of 1% NA/PEEK5％At 588 deg.C, an increase of 18 deg.C by about 3.16%; 3% TiO2Thermal decomposition temperature T of PEEK5％580 ℃ higher by 10 ℃ by about 1.75%; 1% NA/3% TiO2Thermal decomposition temperature T of PEEK5％The highest temperature is 598 ℃, the temperature is increased by 28 ℃, and the temperature is increased by about 4.9 percent, so that the thermal stability of the ternary composite material is greatly improved, and the ternary composite material can be used in a high-temperature harsh environment.
The improvement of the thermal stability of the ternary composite material comes from the thermal reinforcement effect of the nano particles on the material, the movement of polymer chain segments is hindered to a certain extent by the addition of the nano particles, and the transportation of degradation products of most polymers is effectively prevented, so that the thermal degradation process is slowed down.
Claims (6)
1. The polyether-ether-ketone composite material is characterized by being prepared from the following raw materials in percentage by weight: 90-96% of polyether ether ketone, 1-3% of nano-diamond alkene and 251-7% of nano-titanium dioxide, wherein the nano-diamond alkene consists of nano-diamond alkene with the granularity of 50nm, 100nm, 200nm and 250nm, and the mass ratio of the nano-diamond alkene with the granularity of 50nm, 100nm, 200nm and 250nm is (1-2): 2-3): 3-4): 4-5.
2. A method of preparing a polyetheretherketone composite according to claim 1 comprising the steps of:
1) mixing nano diamond alkene and nano titanium dioxide P25 according to the mass ratio of (1-3): 1-7 to obtain a mixture A;
2) stirring and mixing deionized water and the mixture A obtained in the step 1) for 25-35min at an ultrasonic frequency of 40-60 KHz and a stirring rotation speed of 30-60 rpm, then continuously adding 3-aminopropyltriethoxysilane at 65-75 ℃, reacting for 3-4h, centrifuging, drying a centrifugal product, performing heat treatment, and cooling to obtain a modified mixture B, wherein the dosage ratio of the deionized water to the mixture A to the 3-aminopropyltriethoxysilane is 100 mL: 1 g: 6mL, performing four-stage step heating on the heat treatment, and performing heat preservation for 30min after the temperature of a first stage is raised from normal temperature to 60 ℃; in the second stage, the temperature is increased from 60 ℃ to 120 ℃, and then the temperature is kept for 1 h; in the third stage, the temperature is increased from 120 ℃ to 280 ℃, and then the temperature is kept for 3 hours; after the temperature of the fourth stage is increased from 280 ℃ to 400 ℃, the heat is preserved for 10 hours, and the heating rate is 2-3 ℃/min in the heating process of each stage;
3) and (3) mixing the modified mixture B obtained in the step 2) with the polyether-ether-ketone, performing melt extrusion, drying, and performing injection molding to obtain the polyether-ether-ketone composite material.
3. The method of preparing a polyetheretherketone composite according to claim 2, wherein step 2) centrifugation conditions: the centrifugal speed is 4000-8000 rpm, and the centrifugal time is 10-15 min; drying conditions are as follows: the drying temperature is 60-80 ℃, and the drying time is 4-12 h.
4. The method for preparing the polyetheretherketone composite material according to claim 2, wherein the modified mixture B in the step 3) is mixed with polyetheretherketone, and the mixture is placed in an SHR high-speed mixer, and stirred for 6-10 min at a stirring power of 42KW and a stirring speed of 1050 rpm.
5. The method for preparing the polyetheretherketone composite material according to claim 2, wherein in the step 3), a micro-mixing rheometer is adopted for melt extrusion, the processing temperature is 370-395 ℃, and the screw rotation speed is 50-80 rpm; step 3) drying conditions: the drying temperature is 120 ℃, and the drying time is 10 h.
6. The method for preparing polyetheretherketone composite material according to claim 2, wherein the nano-diamond alkene and nano-titanium dioxide P25 in step 1) are mixed and placed in an SHR high-speed mixer, and stirred for 6-10 min at a stirring power of 42KW and a stirring speed of 1050 rpm.
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