CN100348652C - Novel self-lubricating polymer composite material and its prepn process - Google Patents
Novel self-lubricating polymer composite material and its prepn process Download PDFInfo
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- CN100348652C CN100348652C CNB2006100188001A CN200610018800A CN100348652C CN 100348652 C CN100348652 C CN 100348652C CN B2006100188001 A CNB2006100188001 A CN B2006100188001A CN 200610018800 A CN200610018800 A CN 200610018800A CN 100348652 C CN100348652 C CN 100348652C
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Abstract
The present invention relates to a novel composite macromolecular self-lubricating material and a preparation method thereof. The composite material is prepared from 10 to 25 portions by weight of calcium carbonate whisker, 10 portions by weight of polytetrafluoroethylene and 65 to 80 portions by weight of polyetheretherketone. The preparation method comprises the following steps: the raw materials are dried and mixed at a temperature of 130 to 150 DEG C and are put into a stirrer for stirring at a high speed; then, the raw materials are put into a mould cavity of a hot-pressing mould for melting; pressure of 20MPa is added for shaping the materials, and the pressure is kept for 8 to 10 minutes; afterwards, the temperature of the materials is decreased along with the mould to 100 DEG C, and the materials are demoulded, cooled to a room temperature, and thermally insulated at a temperature of 250 DEG C for 1 hour. The present invention aims to use the calcium carbonate whiskers to strengthen the polyetheretherketone, use the polytetrafluoroethylene as an antifriction agent so as to exert the cooperative coupling action among a polyetheretherketone substrate, the calcium carbonate whiskers and the antifriction agent and realize self-lubricating antifriction and abrasive resistance. Accordingly, the novel high-strength self-lubricating composite material can be obtained and has the advantages of small friction coefficient, low abrasion rate, strong bearing capacity, low cost, etc.
Description
Technical field
The present invention relates to common filled high polymer self-lubricating composite of a kind of calcium carbonate crystal whisker and tetrafluoroethylene and preparation method thereof.
Background technology
The many friction duty conditions that with aerospace are the military project high-tech sector of representative have surmounted common operating limit, therefore need seek new high strength anti-friction wear-resistant self-lubricating material adapting to complex operating environment, and the civil engineering field needs also high-performance oil-free lubricatoin friction materials to be proposed requirements at the higher level based on usage environment, energy-conserving and environment-protective, cleaner production etc.Working conditionss such as that macromolecule self-lubricating composite can adapt to is unlubricated, moist, pollution, burn into radiation, its use temperature and supporting capacity also improve constantly, with advantages such as its outstanding performance, price, moulding processs at the show strong application potential in these fields.High performance engineering plastics becomes the critical material that advanced country payes attention to development with specific functions such as excellent properties such as its light weight, intensity height and light, electricity, magnetic, self-lubricatings, has widespread use in Aeronautics and Astronautics, weapons, automobile, machinery, chemical industry, boats and ships, building, technical field such as electric.
Present existing a kind of macromolecule resin material, be polyether-ether-ketone (PEEK), it is a kind of thermoplastic special engineering plastic of all aromatic hemicrystalline, owing to contain the inflexible phenyl ring on the macromolecular chain, the carbonyl of submissive ehter bond and raising Intermolecular Forces, compound with regular structure, has high strength, high tenacity, insulativity, radiation hardness, excellent comprehensive performance such as corrosion-resistant, especially thermotolerance and tribological property are good than the common engineering plastics, and excellent machinability with thermoplastic polymer, be convenient to precise forming, but as tribological material, its second-order transition temperature (Tg) and load heat-drawn wire (being 135-160 ℃) are high not enough, reach more than 0.4 even 0.6 with steel frictional coefficient when rubbing, wear rate is higher, and supporting capacity is limited; In addition, also exist cost than problems such as height.
Pure polyether-ether-ketone tribology research shows, polyether-ether-ketone and steel wear surface when rubbing occur many tangible scraping ditch dug with a plows and scratch and area bigger peel off the hole, the surface of friction pair sticking action makes material time top layer crack initiation under cycle shearing stress effect form fatigue-stripping with expansion layer to wear and tear, and friction process generation temperature rise causes the polyether-ether-ketone skin-material softening, be easy to generate pyroplastic deformation and mobile, plow and adhesion have been increased the weight of again, cause frictional force and frictional coefficient bigger, the fret wear rate is than higher.
Therefore, need in actual use the polyether-ether-ketone enhancing modified with over-all propertieies such as the tribology that improves polyether-ether-ketone, machinery, calorifics.In metal to-metal contact, high temperature, radiation, corrosion etc. under the extreme and bad working environments condition, require polymer composites to have performances such as outstanding self-lubricating maintenance-free performance, frictional coefficient are lower, high temperature resistant, anticorrosive, thereby reduce the friction process temperature rise, improve the material supporting capacity, avoid material surface to produce softening too early and pyroplastic deformation, reduction fret wear rate, improve the life-span.Although modification mode such as traditional fiber reinforcement and nano particle are compound, can be to the antifriction of polyether-ether-ketone based high molecular matrix material, wear-resisting tribological property and the machinery of waiting, the improvement in various degree of realization in a certain respect of performances such as calorifics, but as tribological material, these modification mode also exist as frictional coefficient higher, wear resistance improves remarkable inadequately, correlated performances such as mechanics calorifics are difficult to optimize coupling and the difficult control of complex process, problems such as processability difference, add the high price of packing material itself, the cost of matrix material is risen, hindered its application as self-lubricating composite.
Summary of the invention
In order to address the above problem, the invention provides a kind of macromolecule self-lubricating composite and preparation method thereof, its objective is with lime carbonate (CaCO
3) whisker reinforced polyether ether ketone (PEEK), with polytetrafluoroethylene (PTFE) as low friction compound, collaborative coupling between performance polyether-ether-ketone matrix, calcium carbonate crystal whisker, the low friction compound, the realization self-lubricating antifriction is wear-resisting, and frictional coefficient is little, wear rate is low, supporting capacity is strong, a kind of novel strnegth self-lubricating composite material for high of low cost and other advantages thereby obtain to have.
Technical scheme of the present invention is as follows:
1. macromolecule self-lubricating composite is characterized in that, it comprises the composition of raw materials of following parts by weight: 10～25 parts of calcium carbonate crystal whiskers, 10 parts of tetrafluoroethylene, 65～80 parts of polyether-ether-ketones.
2. the preparation method of macromolecule self-lubricating composite is characterized in that, comprises following preparation steps:
(a) with calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone raw material under 130～150 ℃ of temperature dry 3～5 hours;
(b) get the dried calcium carbonate crystal whisker of step (a), tetrafluoroethylene, polyether-ether-ketone raw material and mix after, put into stirrer, be not less than under the rotating speed of 1000rpm high-speed stirring in speed of rotation and mix 8～10min;
(c) after the material after step (b) is stirred was put into the fusion of 380～390 ℃ of hot pressing die die cavitys, the 20Mpa that pressurizes made forming materials, and after pressurize 8～10min, when being cooled to 100 ℃ with mould, the demoulding is cooled to room temperature;
(d) the cooled material of step (c) demoulding is incubated 1 hour under 250 ℃ of temperature, makes product.
Than prior art, the present invention adopts lime carbonate (CaCO
3) whisker and polytetrafluoroethylene (PTFE) fill polyether-ether-ketone (PEEK) jointly, therefore has following advantage:
(1) since calcium carbonate crystal whisker have high temperature resistant, intensity is high, abrasion performance, anticorrosive, with excellent comprehensive performances such as polymkeric substance avidity is strong, its yardstick circle is between fiber and nano particle, have the active effect of the enhancement and the small sized particles of like fibrous concurrently, therefore, behind the calcium carbonate filled whisker, brought into play the micro-enhancement of calcium carbonate crystal whisker to resin, improved the supporting capacity of polyether-ether-ketone composite material, whisker partly replaces the matrix resin carrying in the friction process, reduce the surface of friction pair adhesion, stoped the pyroplastic deformation of matrix resin.Add tetrafluoroethylene simultaneously, the synergy of tetrafluoroethylene and calcium carbonate crystal whisker obviously reduces the frictional coefficient of lime carbonate/tetrafluoroethylene/polyether-ether-ketone composite material and wear rate.The polyether-ether-ketone molecule has pelletizing shape structure, they are joined together to form fascircular texture, when polyether-ether-ketone slides along the steel surface, the neat degree that arrange along slip direction in the crystal zone of pencil molecular structure is not so good as tetrafluoroethylene, the transfer film that produces on the steel surface is thicker usually and all even inadequately continuous, makes that also pure polyether-ether-ketone frictional coefficient and wear rate are higher.And the tetrafluoroethylene molecule has slick molecule pattern, do not contain branch and do not form intersecting chain yet, when it slides along steel is surperficial, the crystal zone is tended to arrange along slip direction gradually, because the clinging power between the surface makes several layers tetrafluoroethylene molecule transfer to the steel surface gradually, form transfer film subsequently.Tetrafluoroethylene in the macromolecule self-lubricating composite of the present invention exists preferential adhesion with respect to polyether-ether-ketone and shifts, and helps to form even, successive transfer film on antithesis steel loop surface.This smooth contact condition in the friction process between the antithesis surface effectively reduces the frictional coefficient and the wear rate of matrix material.This macromolecule self-lubricating composite has satisfied the many working condition requirements in the engineering field, service requirements under the extreme and bad working environments condition such as especially metal to-metal contact, boundary lubrication, high temperature, radiation, corrosion, the working reliability and the work-ing life of equipment have been improved, reduce the lubricated maintenance expense, for equipment realize microminiaturized, at a high speed, heavy duty and automatically control etc. created favourable condition, also provide the high-performance self-lubricating antifriction high-abrasive material that adapts to the special operation condition requirement for Gao Xinmin recruitment journey fields such as sophisticated technology such as space flight, military affairs and machinery, chemical industry, biologies.
(2) because the abundant raw material of calcium carbonate crystal whisker, synthesis technique is simple, cost is very cheap, have high performance price ratio as the strongthener of polyether-ether-ketone, greatly reduce production cost, its application potential is huge.
(3) macromolecule self-lubricating composite that makes of the present invention can be used for producing tribology associated materials such as bearing and retainer, gear, ring gear, valve, bearing shell axle bush, sealing, push rod, engine part, wide adaptability, can satisfy the service requirements under the bad working environments conditions such as many working condition requirements, especially metal to-metal contact in the engineering field, boundary lubrication, high temperature, radiation, corrosion.
Embodiment
Macromolecule self-lubricating composite of the present invention is characterised in that it comprises the composition of raw materials of following parts by weight: 10～25 parts of calcium carbonate crystal whiskers, 10 parts of tetrafluoroethylene, 65～80 parts of polyether-ether-ketones.The length-to-diameter ratio of described calcium carbonate crystal whisker is between 20～30, and density is 2.86g/cm
3The granularity of described tetrafluoroethylene is 10 μ m, and density is 2.18g/cm
3The density of described polyether-ether-ketone is 1.32g/cm
3, granularity is 100 μ m.
The preparation method of above-mentioned macromolecule self-lubricating composite is characterised in that, comprises following preparation steps:
(a) with calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone raw material under 130～150 ℃ of temperature dry 3～5 hours;
(b) get the dried calcium carbonate crystal whisker of step (a), tetrafluoroethylene, polyether-ether-ketone raw material and mix after, put into stirrer, be not less than under the rotating speed of 1000rpm high-speed stirring in speed of rotation and mix 8～10min;
(c) after the material after step (b) is stirred was put into the fusion of 380～390 ℃ of hot pressing die die cavitys, the 20Mpa that pressurizes made forming materials, and after pressurize 8～10min, when being cooled to 100 ℃ with mould, the demoulding is cooled to room temperature;
(d) the cooled material of step (c) demoulding is incubated 1 hour under 250 ℃ of temperature, makes product.
The present invention is further illustrated with comparison below by specific embodiment, but the present invention is not limited in these examples.
Embodiment 1 (preferred embodiment)
Get 10 parts of raw material calcium carbonate crystal whiskers, 10 parts of tetrafluoroethylene, 80 parts of polyether-ether-ketones, wherein the length-to-diameter ratio of calcium carbonate crystal whisker is 30, density is 2.86g/cm
3, granularity 10 μ m, the density 2.18g/cm of tetrafluoroethylene
3, the density of polyether-ether-ketone is 1.32g/cm
3, granularity 100 μ m, by the preparation of following step:
(a) with calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone raw material under 130 ℃ of temperature dry 5 hours;
(b) get the dried calcium carbonate crystal whisker of step (a), tetrafluoroethylene and polyether-ether-ketone raw material and mix after, put into stirrer, be not less than under the rotating speed of 1000rpm high-speed stirring in speed of rotation and mix 8min;
(c) after the material after step (b) is stirred was put into the fusion of 380 ℃ of hot pressing die die cavitys, the 20Mpa that pressurizes made forming materials, and after the pressurize 8min, when being cooled to 100 ℃ with mould, the demoulding is cooled to room temperature;
(d) the cooled material of step (c) demoulding is incubated 1 hour under 250 ℃ of temperature, makes product.
Embodiment 2 (preferred embodiment)
Get 15 parts of raw material calcium carbonate crystal whiskers, 10 parts of tetrafluoroethylene, 75 parts of polyether-ether-ketones, wherein the length-to-diameter ratio of calcium carbonate crystal whisker is 25, density is 2.86g/cm
3, granularity 10 μ m, the density 2.18g/cm of tetrafluoroethylene
3, the density of polyether-ether-ketone is 1.32g/cm
3, granularity 100 μ m, by the preparation of following step:
(a) with calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone raw material under 140 ℃ of temperature dry 4 hours;
(b) get the dried calcium carbonate crystal whisker of step (a), tetrafluoroethylene and polyether-ether-ketone raw material and mix after, put into stirrer, be not less than under the rotating speed of 1000rpm high-speed stirring in speed of rotation and mix 9min;
(c) after the material after step (b) is stirred was put into the fusion of 385 ℃ of hot pressing die die cavitys, the 20Mpa that pressurizes made forming materials, and after the pressurize 9min, when being cooled to 100 ℃ with mould, the demoulding is cooled to room temperature;
(d) the cooled material of step (c) demoulding is incubated 1 hour under 250 ℃ of temperature, makes product.
Embodiment 3 (preferred embodiment)
Get 20 parts of raw material calcium carbonate crystal whiskers, 10 parts of tetrafluoroethylene, 70 parts of polyether-ether-ketones, wherein the length-to-diameter ratio of calcium carbonate crystal whisker is 25, density is 2.86g/cm
3, granularity 10 μ m, the density 2.18g/cm of tetrafluoroethylene
3, the density of polyether-ether-ketone is 1.32g/cm
3, granularity 100 μ m, by the preparation of following step:
(a) with calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone raw material under 150 ℃ of temperature dry 3 hours;
(b) get the dried calcium carbonate crystal whisker of step (a), tetrafluoroethylene and polyether-ether-ketone raw material and mix after, put into stirrer, be not less than under the rotating speed of 1000rpm high-speed stirring in speed of rotation and mix 10min;
(c) after the material after step (b) is stirred was put into the fusion of 390 ℃ of hot pressing die die cavitys, the 20Mpa that pressurizes made forming materials, and after the pressurize 10min, when being cooled to 100 ℃ with mould, the demoulding is cooled to room temperature;
(d) the cooled material of step (c) demoulding is incubated 1 hour under 250 ℃ of temperature, makes product.
Embodiment 4 (preferred embodiment)
Get 25 parts of raw material calcium carbonate crystal whiskers, 10 parts of tetrafluoroethylene, 65 parts of polyether-ether-ketones, wherein the length-to-diameter ratio of calcium carbonate crystal whisker is 20, density is 2.86g/cm
3, granularity 10 μ m, the density 2.18g/cm of tetrafluoroethylene
3, the density of polyether-ether-ketone is 1.32g/cm
3, granularity 100 μ m, by the preparation of following step:
(a) with calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone raw material under 150 ℃ of temperature dry 3 hours;
(b) get the dried calcium carbonate crystal whisker of step (a), tetrafluoroethylene and polyether-ether-ketone raw material and mix after, put into stirrer, be not less than under the rotating speed of 1000rpm high-speed stirring in speed of rotation and mix 10min;
(c) after the material after step (b) is stirred was put into the fusion of 390 ℃ of hot pressing die die cavitys, the 20Mpa that pressurizes made forming materials, and after the pressurize 10min, when being cooled to 100 ℃ with mould, the demoulding is cooled to room temperature;
(d) the cooled material of step (c) demoulding is incubated 1 hour under 250 ℃ of temperature, makes product.
The contrast experiment:
Getting pure polyether-ether-ketone (PEEK) is sample one, the sample of embodiment 1 is a sample two, the sample of embodiment 2 is a sample three, the sample of embodiment 3 is a sample four, the sample of embodiment 4 is a sample five, carries out the friction and wear behavior determination test on MM200 type trier, and the friction pair way of contact is the contact of ring-piece, block sample is fixed, and the even part of following ring is the quenching 45 of diameter 40mm
#Steel loop, Rockwell hardness 50HRC, surfaceness 0.3 μ m.Specimen surface is with No. 900 liquid honings before the test, and clean with acetone.Test load 196N, sliding velocity 0.44m/s, wearing-in period 120min, combined stroke are 3168m.Test conditions is the room temperature metal to-metal contact.Frictional coefficient is got the frictional coefficient mean value of the stable back 60min of Frotteurism.Wear rate is the wear volume loss [unit 10 on per unit load and the sliding distance
-6Mm
3(Nm)
-1].Ultimate bearing capacity is final destructive ultimate load, and the load when frictional coefficient or wear rate sudden change promptly occurring in loading procedure step by step is considered as utmost carrying ability.The result of test frictional coefficient, wear rate, supporting capacity contrasts as shown in table 1.
Table 1: the comparison of test results of the frictional coefficient of various sample, wear rate and ultimate bearing capacity
| Test piece number (Test pc No.) | Sample one | Sample two | Sample three | Sample four | Sample five |
| Frictional coefficient | 0.42 | 0.27 | 0.26 | 0.26 | 0.25 |
| Wear rate [10 -6mm 3(Nm) -1] | 9.16 | 0.48 | 0.35 | 0.33 | 1.63 |
| Ultimate bearing capacity (N) | 800 | 1700 | 1800 | 2000 | 1600 |
As seen from Table 1, calcium carbonate filled whisker and tetrafluoroethylene can obviously reduce the frictional coefficient of polymer matrix composites, and along with calcium carbonate crystal whisker content increases, friction coefficient of composite material continues to reduce.When the content proportioning of calcium carbonate crystal whisker, tetrafluoroethylene, polyether-ether-ketone was 25: 10: 65, the frictional coefficient of matrix material was 0.25, reduced significantly than 0.42 of pure polyether-ether-ketone.Calcium carbonate filled whisker and tetrafluoroethylene also make the wear resistance of polyether-ether-ketone composite material obviously improve, and the wear rate of matrix material descends with the whisker adding.When the content proportioning of calcium carbonate crystal whisker, tetrafluoroethylene, polyether-ether-ketone was 15: 10: 75, the wear rate of matrix material had only 1/26 of pure polyether-ether-ketone wear rate.When the content proportioning of calcium carbonate crystal whisker, tetrafluoroethylene, polyether-ether-ketone was 20: 10: 70, the wear rate of matrix material had only 1/27 of pure polyether-ether-ketone wear rate.The ultimate bearing capacity of the polyether-ether-ketone composite material that calcium carbonate crystal whisker and tetrafluoroethylene are filled increases substantially than pure polyether-ether-ketone, when the content proportioning of calcium carbonate crystal whisker, tetrafluoroethylene, polyether-ether-ketone was 20: 10: 70, the ultimate bearing capacity of matrix material was 2.5 times of pure polyether-ether-ketone.
The polyetheretherketoneself self-lubricating hard matrix material that above-mentioned analysis revealed calcium carbonate crystal whisker and tetrafluoroethylene are filled significantly improves than comprehensive tribological properties such as the antifriction of pure polyether-ether-ketone, wear-resisting, supporting capacitys.
The present invention is not limited to the assembly and the preparation method of the foregoing description, also can adopt other assembly and preparation method in the specific implementation, as long as utilize calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone to come assembly and preparation as the component of matrix material.
Claims (3)
1. a macromolecule self-lubricating composite is characterized in that, it comprises the composition of raw materials of following parts by weight: 10～25 parts of calcium carbonate crystal whiskers, 10 parts of tetrafluoroethylene, 65～80 parts of polyether-ether-ketones.
2. macromolecule self-lubricating composite according to claim 1 is characterized in that: the length-to-diameter ratio of described calcium carbonate crystal whisker is between 20～30, and density is 2.86g/cm
3The granularity of described tetrafluoroethylene is 10 μ m, and density is 2.18g/cm
3The density of described polyether-ether-ketone is 1.32g/cm
3, granularity is 100 μ m.
3. the preparation method of a macromolecule self-lubricating composite according to claim 1 and 2 is characterized in that, comprises following preparation steps:
(a) with calcium carbonate crystal whisker, tetrafluoroethylene and polyether-ether-ketone raw material under 130～150 ℃ of temperature dry 3～5 hours;
(b) get the dried calcium carbonate crystal whisker of step (a), tetrafluoroethylene, polyether-ether-ketone raw material and mix after, put into stirrer, be not less than under the rotating speed of 1000rpm high-speed stirring in speed of rotation and mix 8～10min;
(c) after the material after step (b) is stirred was put into the fusion of 380～390 ℃ of hot pressing die die cavitys, the 20Mpa that pressurizes made forming materials, and after pressurize 8～10min, when being cooled to 100 ℃ with mould, the demoulding is cooled to room temperature;
(d) the cooled material of step (c) demoulding is incubated 1 hour under 250 ℃ of temperature, makes product.
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| CN100398605C (en) * | 2006-11-02 | 2008-07-02 | 南京工业大学 | Titanium base whisker reinforced polyether ether ketone wearable composite material and its preparation method |
| CN103013090A (en) * | 2011-09-21 | 2013-04-03 | 重庆信合塑胶有限公司 | Polyaryletherketone composite material and application of the same in bridge bearing |
| CN102504478B (en) * | 2011-11-24 | 2013-06-26 | 东北石油大学 | Porous-grade polyether-ether-ketone self-lubricating wear-resistant composite material and preparation method thereof |
| CN103410848B (en) * | 2013-07-18 | 2016-03-30 | 西北工业大学 | Creep-resistant composite material thrust washer and preparation method thereof |
| CN103486262A (en) * | 2013-09-17 | 2014-01-01 | 常州君华特种工程塑料制品有限公司 | Polyether-ether-ketone sealing partition for filter unit in petroleum industry and manufacturing method |
| CN105504763B (en) * | 2014-09-23 | 2018-06-15 | 株洲时代新材料科技股份有限公司 | Whisker reinforcement polyether-ether-ketone composite material and preparation method thereof |
| CN105061990B (en) * | 2015-09-28 | 2017-06-16 | 吉林大学 | A kind of sulfonation hyperbranched polyarylether ketone modified calcium carbonate whisker/polyether-ether-ketone composite material and preparation method thereof |
| CN105524417A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Potassium titanate whisker reinforced PEEK/PTFE resin and preparation method thereof |
| CN105524410A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Calcium carbonate whisker reinforced PEEK/PTFE resin and preparation method thereof |
| CN105542388A (en) * | 2015-11-03 | 2016-05-04 | 南京肯特复合材料有限公司 | Potassium titanate whisker reinforced PEEK/PTFE composite material and preparation method thereof |
| CN105524409A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Potassium titanate whisker reinforced PEEK composite material and preparation method thereof |
| CN109135174A (en) * | 2017-06-16 | 2019-01-04 | 合肥杰事杰新材料股份有限公司 | A kind of rigidity-toughness balanced polyether-ether-ketone composite material and preparation method thereof |
| CN111286154A (en) * | 2020-03-20 | 2020-06-16 | 中国科学院兰州化学物理研究所 | Flaky silver-coated copper filled polyetheretherketone wear-resistant composite material and preparation method thereof |
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