CN1168781C - Self-lubricating nano composite material and its preparation method - Google Patents
Self-lubricating nano composite material and its preparation method Download PDFInfo
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- CN1168781C CN1168781C CNB021501807A CN02150180A CN1168781C CN 1168781 C CN1168781 C CN 1168781C CN B021501807 A CNB021501807 A CN B021501807A CN 02150180 A CN02150180 A CN 02150180A CN 1168781 C CN1168781 C CN 1168781C
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Abstract
The present invention relates to a nanometer compound material and a preparation method thereof, particularly to a self-lubrication nanometer compound material and a preparation method thereof. The material is prepared from the components of the following shares by weight: 100 shares of fusible polyimide, 1 to 25 shares of inorganic nanometer, 0.1 to 2 shares of coupling agent and 5 to 30 shares of carbon filament. The compound material is applicable to the special environments of vacuum, radiation, high temperature, etc., and is applicable to the self-lubricating bearings, the gear wheels and other components of aerospace, machinery, the chemical industry, automobiles, household appliances and other fields.
Description
Technical field
The present invention relates to a kind of nano composite material and preparation method thereof, particularly a kind of self-lubricating nano-composite material and preparation method thereof.
Background technology
Filler strengthens polymer composite and is widely used in many industries, has solved many great technical barriers.And nano material has had more research and application with its unique character in metal, stupalith field, and the development in the high molecular polymer field still belongs to starting; At present both at home and abroad the polymer based nanocomposites of report mainly is that the direct blending with polymer solids and inorganic nano is many, nanoparticle is difficult to reach ideal uniform and disperses in polymeric matrix, influence the interface bonding of nanoparticle and polymeric matrix.For this reason, Chinese patent CN1258690A has reported the preparation method of polyimide/clay nano composite membrane, can obtain having the film of super-low expansion coefficient; Chinese patent CN1227234A has reported in the suspension system of polymer beads original position and has generated the method that nano zirconium dioxide prepares polymer nanocomposites, and this method can be improved the tribological property of existing polymer composites; But these two patents all do not relate to relevant nano-silicon nitride, nano silicon, carbon nanotube and add in the performed polymer of ANALYSIS OF MOLDABLE POLYIMIDES and carry out compound study on the modification and application report, and this method can effectively improve the dispersion of nanoparticle in polymeric matrix, thereby effectively strengthens the performance of nano composite material.Such nano composite material is formed its tribological property of consideration as high temperature resistant self-lubricating material from structure, does not also see document and patent report as yet.
Summary of the invention
The object of the present invention is to provide a kind of self-lubricating nano-composite material and preparation method thereof.
The present invention realizes by following measure:
A kind of self-lubricating nano-composite material is characterized in that the parts by weight of material are made up of 100 parts of ANALYSIS OF MOLDABLE POLYIMIDES, inorganic nano 1-25 part, coupling agent 0.1-2 part and carbon fiber 5-30 part; The molecular structural formula of polyimide matrix is suc as formula (I).
Inorganic nano select for use in nano-silicon nitride, nano silicon, the carbon nanotube a kind of, two or three.
Coupling agent of the present invention is selected γ-(methacryloxypropyl) propyl trimethoxy silicane for use.
The diameter of nano-silicon nitride, nano silicon dioxide particles is less than 80nm, and the carbon nanotube caliber is less than 100nm.
The used carbon fiber of the present invention is long to be 40-100 μ m.
As polymeric matrix, homodisperse inorganic nano-particle is in order to improve the friction and wear behavior of body material with ANALYSIS OF MOLDABLE POLYIMIDES in the present invention; Carbon fiber can improve the physical and mechanical properties and the tribological property of matrix material as properties-correcting agent.
The preparation method of self-lubricating nano-composite material is characterized in that this method may further comprise the steps successively:
A. inorganic nano 1-25 part, coupling agent 0.1-2 part and organic solvent 100-300 part are mixed, join in 100 parts the performed polymer polyamic acid of ANALYSIS OF MOLDABLE POLYIMIDES, logical nitrogen, drying, stirring add carbon fiber 5-30 part then, stir again;
B. adopt heating or adding pyridine, aceticanhydride or tertiary amine as the method for precipitation agent matrix material to be precipitated out, drying obtains the polyimide nano-composite material powder;
C. during matrix material is packed mould into, be forced into 3-20Mpa, be warming up to 300-360 ℃, be incubated 10-60 minute, be forced into 10-80Mpa, cool off the demoulding under the pressurize condition.
The used organic solvent of the present invention is one or more in dimethyl formamide, N,N-DIMETHYLACETAMIDE, N-Methyl pyrrolidone, the meta-cresol.
The main performance index of matrix material of the present invention is as follows:
1. outward appearance: no significant defect
2. density:＜2.4g/cm
3
3. bending strength:＞130Mpa
4. microhardness (HV): 45～60
5. frictional coefficient:＜0.25 (GB3960-83)
6. abrasion resistance:＜1.8 * 10
-6Mm
3/ (N.m) (GB3960-83)
The present invention compared with prior art has following substantial advantage:
Inorganic nano-particle obtains homodisperse in the matrix material of the present invention, and the adding of properties-correcting agent when improving the ANALYSIS OF MOLDABLE POLYIMIDES friction and wear behavior, does not reduce the physical strength of material; Can be used as the self-lubricating moving parts under the big PV value DRY SLIDING, owing to radioprotective, the good heat resistance of matrix material, can be used on some parts of aerospace field simultaneously.This material can be widely used on the moving parts in fields such as aerospace, mechanical chemical industry, household electrical appliances microcomputer.
Embodiment
Embodiment 1:
With polyamic acid 10g, add 0.1g coupling agent and solvent N-Methyl pyrrolidone among nano silicon nitride 0.5g, nano silicon 0.2g, the carbon nanotube 0.1g, after ultrasonication was uniformly dispersed in 15 minutes, add in the polyamic acid system, logical nitrogen, drying, mechanical stirring 7 hours, add carbon fiber 1.2g, fully stirred again 3 hours.Go out matrix material with the heating method rapid precipitation, in vacuum drying oven, handled 3 hours in 245 ℃, dried matrix material is packed in the mould, be forced into 15Mpa, the heat-up rate with 6 ℃/min rises to 340 ℃ then, constant temperature 25 minutes, be forced into 40Mpa, cool off the demoulding under the pressurize condition.
Embodiment 2:
With polyamic acid 9g, add 0.2g coupling agent and solvent N-Methyl pyrrolidone among nano silicon nitride 0.6g, nano silicon 0.2g, the carbon nanotube 0.2g, after ultrasonication was uniformly dispersed in 20 minutes, add in the polyamic acid system, logical nitrogen, drying, mechanical stirring 8.5 hours, add carbon fiber 2g, fully stirred again 4 hours.Go out matrix material with pyridine, aceticanhydride rapid precipitation, in vacuum drying oven, handled 4 hours in 240 ℃, dried matrix material is packed in the mould, be forced into 20Mpa, the heat-up rate with 6 ℃/min rises to 330 ℃ then, constant temperature 40 minutes, be forced into 50Mpa, cool off the demoulding under the pressurize condition.
Embodiment 3:
With polyamic acid 17.6g, add 0.15g coupling agent and solvent N-Methyl pyrrolidone among nano-silicon nitride 1g, the carbon nanotube 0.6g, after ultrasonication was uniformly dispersed in 18 minutes, add in the polyamic acid system, logical nitrogen, drying, mechanical stirring 10 hours, add carbon fiber 2.7g, fully stirred again 4 hours.Go out matrix material with pyridine, aceticanhydride rapid precipitation, in vacuum drying oven, handled 3 hours in 250 ℃, dried matrix material is packed in the mould, be forced into 20Mpa, the heat-up rate with 6 ℃/min rises to 350 ℃ then, constant temperature 20 minutes, be forced into 60Mpa, cool off the demoulding under the pressurize condition.
Embodiment 4:
With polyamic acid 12.55g, add 0.1g coupling agent and solvent N-Methyl pyrrolidone among the nano-silicon nitride 0.97g, after ultrasonication was uniformly dispersed in 10 minutes, add in the polyamic acid system, logical nitrogen, drying, mechanical stirring 7 hours add carbon fiber 1.9g, fully stir 4 hours again.Go out matrix material with pyridine, aceticanhydride rapid precipitation, in vacuum drying oven, handled 2 hours in 260 ℃, dried matrix material is packed in the mould, be forced into 15Mpa, the heat-up rate with 6 ℃/min rises to 335 ℃ then, constant temperature 40 minutes, be forced into 50Mpa, cool off the demoulding, processing sample preparation under the pressurize condition.
Claims (6)
1, a kind of self-lubricating nano-composite material is characterized in that the parts by weight of material consist of: 100 parts of ANALYSIS OF MOLDABLE POLYIMIDES, inorganic nano 1-25 part, coupling agent 0.1-2 part and carbon fiber 5-30 part; The molecular structural formula of polyimide matrix is suc as formula (I)
Inorganic nano select for use in nano-silicon nitride, nano silicon, the carbon nanotube a kind of, two or three.
2,, it is characterized in that coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane as the said material of claim 1.
3, as the said material of claim 1, the diameter that it is characterized in that nano-silicon nitride, nano silicon dioxide particles is less than 80nm, and the carbon nanotube caliber is less than 100nm.
4,, it is characterized in that the long 40-100 μ m of being of carbon fiber as the said material of claim 1.
5, a kind of preparation method of self-lubricating nano-composite material, this method may further comprise the steps successively:
A. inorganic nano 1-25 part, coupling agent 0.1-2 part and organic solvent 100-300 part are mixed, join in 100 parts the performed polymer polyamic acid of ANALYSIS OF MOLDABLE POLYIMIDES, logical nitrogen, drying, stirring add carbon fiber 5-30 part then, stir again;
B. adopt heating or adding pyridine, aceticanhydride or tertiary amine as the method for precipitation agent matrix material to be precipitated out, drying obtains the polyimide nano-composite material powder;
C. during matrix material is packed mould into, be forced into 3-20Mpa, be warming up to 300-360 ℃, be incubated 10-60 minute, be forced into 10-80Mpa, cool off the demoulding under the pressurize condition.
6,, it is characterized in that organic solvent is one or more in dimethyl formamide, N,N-DIMETHYLACETAMIDE, N-Methyl pyrrolidone, the meta-cresol as the said method of claim 5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021501807A CN1168781C (en) | 2002-11-15 | 2002-11-15 | Self-lubricating nano composite material and its preparation method |
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| CNB021501807A CN1168781C (en) | 2002-11-15 | 2002-11-15 | Self-lubricating nano composite material and its preparation method |
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| CN1168781C true CN1168781C (en) | 2004-09-29 |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2263971A1 (en) * | 2009-06-09 | 2010-12-22 | Nivarox-FAR S.A. | Composite micromechanical part and method for manufacturing same |
| CN102181153B (en) * | 2011-03-30 | 2013-04-17 | 同济大学 | Preparation method of carbon nanotube/functionalized carbon fiber reinforced polyimide composite material |
| CN103122145A (en) * | 2011-11-18 | 2013-05-29 | 中国科学院兰州化学物理研究所 | Self-lubrication composite material of polyimide |
| CN102931149B (en) * | 2012-11-15 | 2015-06-03 | 中国科学院深圳先进技术研究院 | Nano-silicon dioxide and nano-silicon nitride composite material and preparation method thereof |
| CN103554909B (en) * | 2013-10-22 | 2015-10-21 | 中国科学院深圳先进技术研究院 | Carbon nano tube compound material, its preparation method, prepreg and copper-clad base plate that polymer-silica is coated |
| CN105368047A (en) * | 2015-10-15 | 2016-03-02 | 丽水市高升科技有限公司 | Material of high strength harmonic reducer cam |
| CN105924965B (en) * | 2016-05-13 | 2018-06-26 | 江苏大学 | A kind of preparation method of anti-friction wear-resistant polymer matrix composite |
| CN106519667A (en) * | 2016-10-11 | 2017-03-22 | 陕西科技大学 | High-temperature-resistant polyamide imide nanometer ultrathin film and preparation method thereof |
| CN106497052A (en) * | 2016-10-11 | 2017-03-15 | 陕西科技大学 | A kind of high temperature resistance polyester imine nanometer ultrathin membrane and preparation method thereof |
| CN107815108B (en) * | 2017-10-24 | 2022-04-12 | 河北省科学院能源研究所 | Ether anhydride type polyimide composite molding material |
| CN107793758B (en) * | 2017-11-15 | 2020-08-07 | 江苏亚宝绝缘材料股份有限公司 | Polymer of carbon nano tube composite polyimide resin and preparation and application thereof |
| CN110355078B (en) * | 2019-07-29 | 2022-05-24 | 大连海事大学 | Method for slowing down release of self-lubricant of packaged solid in surface microtexture |
| CN111286196B (en) * | 2020-03-16 | 2021-02-26 | 中国科学院兰州化学物理研究所 | Self-lubricating fabric liner composite material and preparation method and application thereof |
| CN111978806A (en) * | 2020-09-11 | 2020-11-24 | 湖南尚鑫新材料科技有限公司 | Scratch-resistant heat-resistant coating and preparation method thereof |
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