CN111205592A - Nano titanium nitride filled polyether-ether-ketone composite lubricating material and preparation method thereof - Google Patents
Nano titanium nitride filled polyether-ether-ketone composite lubricating material and preparation method thereof Download PDFInfo
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- CN111205592A CN111205592A CN202010221356.3A CN202010221356A CN111205592A CN 111205592 A CN111205592 A CN 111205592A CN 202010221356 A CN202010221356 A CN 202010221356A CN 111205592 A CN111205592 A CN 111205592A
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- titanium nitride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a polyether-ether-ketone composite lubricating material filled with nano titanium nitride, which is prepared by ultrasonically stirring and dispersing polyether-ether-ketone (95-99 wt.%) and nano titanium nitride (1-5 wt.%) in industrial alcohol to prepare mixed powder, pouring the mixed powder into a mold, performing hot press molding at a certain temperature and under a certain pressure, and naturally cooling. The tribological property test result shows that the tribological property of the polymer composite material can be obviously improved by filling a small amount of nano titanium nitride in the polyether-ether-ketone composite material, so that the low friction and high wear resistance of the material are realized, and the application of the nano titanium nitride as a lubricating additive is expanded. In addition, the selected nano titanium nitride has small particle size, large specific surface area, small filling amount, low cost and simple preparation process, and provides a new idea for the design of polymer lubricating materials.
Description
Technical Field
The invention relates to a polyether-ether-ketone composite material, in particular to a polyether-ether-ketone composite lubricating material filled with nano titanium nitride and a preparation method thereof, belonging to the field of composite materials and the technical field of lubricating materials.
Background
The polyetheretherketone is a crystalline thermoplastic engineering plastic with excellent performance, and has the advantages of high temperature resistance, chemical corrosion resistance, creep resistance, excellent electrical insulation performance and the like. However, pure polyetheretherketone materials have a large friction coefficient and poor abrasion resistance, and are difficult to meet the use requirements. In practical application, polyether-ether-ketone is used as a resin matrix, and a solid lubricant, a nano functional filler and the like are filled for modification to prepare the low-friction high-wear-resistance polymer self-lubricating composite material.
The nano functional filler has small size effect, the tribology performance can be obviously improved by filling a small amount of proper nano particles with polymers, and after filling, the abrasive particles can not be worn on the friction surface generally, and the dual surface can not be damaged. In addition, the nano particles falling off from the wear surface can also play a role of a molecular bearing, so that the friction coefficient is obviously reduced. Therefore, the nano-filling polymer composite material has wide application prospect in the field of lubrication and sealing. How to select proper nano particles and optimal filling amount is the key point of the development of the materials.
The nano titanium nitride has the advantages of large specific surface area, high surface activity, high nitrogen content (> 30%), high temperature resistance, oxidation resistance, high hardness, excellent infrared ray absorption performance (more than 80% of ultraviolet light is shielded by more than 85%), good barrier property and good conductivity, and is widely applied to plastic engineering, solar energy absorbers, high-emissivity coatings and the like. The nano titanium nitride can also be used as a reinforcing phase for improving the strength and toughness of metal and ceramic matrixes. However, the application of the lubricating antifriction filler is not published in relevant patents and documents at present.
Disclosure of Invention
The invention aims to provide a nano titanium nitride filled polyether-ether-ketone composite lubricating material and a preparation method thereof.
Preparation of polyether-ether-ketone composite lubricating material filled with nano titanium nitride
The invention relates to a nanometer titanium nitride filled polyether-ether-ketone composite lubricating material, which is prepared from the following raw material components by the process:
the raw material components (by mass percent): 95-99% of polyether-ether-ketone and 1-5% of nano titanium nitride. Wherein the particle size of the polyether-ether-ketone is 75-150 mu m; the particle size of the nano titanium nitride is 10-30 nm;
the preparation process comprises the following steps: the method comprises the following steps:
(1) mixing materials: adding nano titanium nitride into industrial alcohol, ultrasonically stirring for 0.5-1 hour, adding polyether-ether-ketone, continuously ultrasonically stirring for 0.5-1 hour, fully mixing uniformly, performing suction filtration, and drying to obtain mixed powder. The power of an ultrasonic cleaning machine adopted in the ultrasonic mechanical stirring is 500W, and the mechanical stirring speed is 200 rpm;
(2) hot-press molding: pouring the mixed powder into a mould for hot-press molding. The hot-press molding is to keep the temperature and the pressure for 120-150 min at 360-390 ℃ and 10-15 MPa;
(3) and (3) cooling: natural cooling is adopted; and firstly, keeping the pressure of 10-15 MPa until the temperature is reduced to 340 ℃, then keeping the pressure of 20-25 MPa until the temperature is reduced to 280 ℃, then cooling to 140-150 ℃, and demoulding to obtain the polyether-ether-ketone composite lubricating material.
Friction performance test of polyether-ether-ketone composite lubricating material filled with nano titanium nitride
The test method comprises the following steps: GB/T3960, 200N, 200rpm,120 min;
and (3) testing results: friction coefficient less than or equal to 0.28, volumetric wear rate less than or equal to 1 multiplied by 10-5mm3/N.m。
The tribological property test result shows that the tribological property of the polymer composite material can be obviously improved by filling a small amount of nano titanium nitride in the polyether-ether-ketone composite material, so that the low friction and high wear resistance of the material are realized, and the application of the nano titanium nitride as a lubricating additive is expanded. In addition, the selected nano titanium nitride has small particle size, large specific surface area, small filling amount, low cost and simple preparation process, and provides a new idea for the design of polymer lubricating materials.
Detailed Description
The preparation and properties of the polyetheretherketone composite lubricating material of the present invention are further illustrated by the following specific examples.
Example one
1. The raw material ratio is as follows: 99g of polyether-ether-ketone and 1g of nano titanium nitride;
2. the preparation process comprises the following steps:
A. mixing materials: adding nano titanium nitride into industrial alcohol, ultrasonically stirring for 0.5 hour, then adding polyether-ether-ketone, continuously ultrasonically stirring for 0.5 hour, fully and uniformly mixing, and then carrying out suction filtration and drying;
B. hot-press molding: pouring the mixed powder into a mould, and carrying out hot press molding, namely keeping the temperature and the pressure at 360 ℃ and 15MPa for 150 min;
C. and (3) cooling: naturally cooling, maintaining the pressure at 10MPa in the process of reducing the temperature to 340 ℃ at 360 ℃, maintaining the pressure at 20MPa in the process of reducing the temperature to 280 ℃ at 340 ℃, and demoulding at 140 ℃ to obtain the product;
3. the tribological performance indexes are as follows: friction coefficient of 0.27, volumetric wear rate less than or equal to 0.90X 10-5mm3M (GB/T3960, 200N, 200rpm,120 min). Compared with pure polyimide, the friction coefficient is reduced by 15.6%, and the volume wear rate is reduced by 18.9%.
Example two
1. The raw material ratio is as follows: 97g of polyether-ether-ketone and 3g of nano titanium nitride;
2. the preparation process comprises the following steps:
A. mixing materials: adding nano titanium nitride into industrial alcohol, ultrasonically stirring for 0.6 h, then adding polyether-ether-ketone, continuously ultrasonically stirring for 0.6 h, fully and uniformly mixing, and then carrying out suction filtration and drying;
B. hot-press molding: pouring the mixed powder into a mould, and performing hot press molding by keeping the temperature and the pressure at 370 ℃ and 13MPa for 140 min;
C. and (3) cooling: naturally cooling, maintaining the pressure at 15MPa when the temperature is reduced to 340 ℃ at 370 ℃, maintaining the pressure at 25MPa when the temperature is reduced to 280 ℃ at 340 ℃, and demoulding when the temperature is reduced to 150 ℃ to obtain the product;
3. the tribological performance indexes are as follows: friction coefficient of 0.25, volumetric wear rate less than or equal to 0.72 multiplied by 10-5mm3M (GB/T3960, 200N, 200rpm, 20 min). With pure polyimide (coefficient of friction 0.32, volumetric wear rate 1.11X 10)-5mm3N.m), the friction coefficient is reduced by 21.8%, and the volumetric wear rate is reduced by 35.1%.
EXAMPLE III
1. The raw material ratio is as follows: 95g of polyether-ether-ketone and 5g of nano titanium nitride;
2. the preparation process comprises the following steps:
A. mixing materials: adding nano titanium nitride into industrial alcohol, ultrasonically stirring for 0.7 hour, then adding polyether-ether-ketone, continuously ultrasonically stirring for 0.7 hour, fully and uniformly mixing, and then carrying out suction filtration and drying;
B. hot-press molding: pouring the mixed powder into a mould, and carrying out hot press molding by keeping the temperature and the pressure at 375 ℃ and 12MPa for 130 min;
C. and (3) cooling: naturally cooling, maintaining the pressure at 12MPa when the temperature of 375 ℃ is reduced to 340 ℃, maintaining the pressure at 22MPa when the temperature of 340 ℃ is reduced to 280 ℃, and demoulding when the temperature is reduced to 145 ℃ to obtain the product;
3. the tribological performance indexes are as follows: friction coefficient of 0.28, volumetric wear rate less than or equal to 1.0 multiplied by 10-5mm3M (GB/T3960, 200N, 200rpm, 20 min). Compared with pure polyimide, the friction coefficient is reduced by 12.5%, and the volume wear rate is reduced by 9.9%.
In each embodiment, the particle size of the polyether-ether-ketone is 75-150 μm; the particle size of the nano titanium nitride is 10-30 nm.
Claims (6)
1. A nanometer titanium nitride filled polyether-ether-ketone composite lubricating material is prepared from the following raw material components by the following process:
the raw material components are as follows: 95-99 wt.% of polyether-ether-ketone and 1-5 wt.% of nano titanium nitride;
the preparation process comprises the following steps: adding nano titanium nitride into industrial alcohol, ultrasonically stirring for 0.5-1 hour, adding polyether-ether-ketone, continuously ultrasonically stirring for 0.5-1 hour, fully mixing uniformly, performing suction filtration, and drying to obtain mixed powder; and then pouring the mixed powder into a mould for hot-press molding, naturally cooling, demoulding and preparing the polyether-ether-ketone composite lubricating material.
2. The nano titanium nitride-filled polyetheretherketone composite lubricating material of claim 1, wherein: the particle size of the polyether-ether-ketone is 75-150 mu m.
3. The nano titanium nitride-filled polyetheretherketone composite lubricating material of claim 1, wherein: the particle size of the nano titanium nitride is 10-30 nm.
4. The nano titanium nitride-filled polyetheretherketone composite lubricating material of claim 1, wherein: the power of an ultrasonic cleaning machine adopted in the ultrasonic mechanical stirring is 500W, and the mechanical stirring speed is 200 rpm.
5. The nano titanium nitride-filled polyetheretherketone composite lubricating material of claim 1, wherein: the hot-press forming is carried out at the temperature of 360-390 ℃ and under the pressure of 10-15 MPa for 120-150 min.
6. The nano titanium nitride-filled polyetheretherketone composite lubricating material of claim 1, wherein: in the natural cooling process, the pressure is kept at 10-15 MPa until the temperature is reduced to 340 ℃, then the pressure is kept at 20-25 MPa until the temperature is reduced to 280 ℃, then the temperature is reduced to 140-150 ℃, and demoulding is carried out.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106751442A (en) * | 2016-11-11 | 2017-05-31 | 中国科学院兰州化学物理研究所 | A kind of multivariant oxide filling polyether-ether-ketone base self-lubricating nano composite material and preparation method thereof |
| CN107090158A (en) * | 2017-05-09 | 2017-08-25 | 常州德毅新材料科技有限公司 | A kind of wear-resisting polyetheretherketonematerials materials and preparation method thereof |
| CN109021494A (en) * | 2018-06-29 | 2018-12-18 | 南京航空航天大学 | A kind of graphene modified polyether ether ketone composite material and preparation method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106751442A (en) * | 2016-11-11 | 2017-05-31 | 中国科学院兰州化学物理研究所 | A kind of multivariant oxide filling polyether-ether-ketone base self-lubricating nano composite material and preparation method thereof |
| CN107090158A (en) * | 2017-05-09 | 2017-08-25 | 常州德毅新材料科技有限公司 | A kind of wear-resisting polyetheretherketonematerials materials and preparation method thereof |
| CN109021494A (en) * | 2018-06-29 | 2018-12-18 | 南京航空航天大学 | A kind of graphene modified polyether ether ketone composite material and preparation method |
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Application publication date: 20200529 |