CN109401812B - Space solid lubricating coating and preparation method thereof - Google Patents

Space solid lubricating coating and preparation method thereof Download PDF

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CN109401812B
CN109401812B CN201811271734.8A CN201811271734A CN109401812B CN 109401812 B CN109401812 B CN 109401812B CN 201811271734 A CN201811271734 A CN 201811271734A CN 109401812 B CN109401812 B CN 109401812B
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coating
ptfe
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polishing
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CN109401812A (en
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袁兴栋
杨晓洁
刘勇
王泽力
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Shandong Jianzhu University
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M147/00—Lubricating compositions characterised by the additive being a macromolecular compound containing halogen
    • C10M147/02—Monomer containing carbon, hydrogen and halogen only
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C09D127/18—Homopolymers or copolymers of tetrafluoroethene
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/08—Solids

Abstract

The invention discloses a space solid lubricating coating and a preparation method thereof, wherein the coating component of a solid lubricant is PTFE particles with the size of 40-100 meshes, the friction coefficient of the coating is low (0.125-0.185), the abrasion loss is small (0.3-4.8 g), the structure is uniform and continuous, and the thickness is about 20 mu m. The preparation method is scientific and reasonable, and has great achievement transformation potential and wide practical value.

Description

Space solid lubricating coating and preparation method thereof
Technical Field
The invention relates to a lubricating coating and a preparation method thereof, in particular to a space solid lubricating coating and a preparation method thereof.
Background
Space lubricating materials are generally classified into solid lubricating materials and liquid lubricating materials. A commonly used lubricating material for the spaces is a solid lubricating material. Generally, the composite material is divided into four types, namely a substance with a laminated structure, a soft metal, a high polymer material and a self-lubricating composite material. The lubricating material with a laminated structure comprises a transition metal disulfide compound MoS2、WS2、NbSe2And graphite. Wherein MoS2And WS2Most commonly, they have a lower coefficient of friction in vacuum than in air, and their use temperatures in vacuum are higher than in air, which is an ideal space lubricant.
The soft metal used as the solid lubricant mainly comprises gold, silver, lead, zinc and the like, wherein the gold, the silver and the lead exist in a simple substance form, and the three have a face-centered cubic structure, so that the soft metal has the advantages of no low-temperature brittleness and good lubricating property in a low-temperature environment. The polymer material used for the space lubricant is mainly polytetrafluoroethylene, polyimide, phenolic resin, epoxy resin and the like, and compared with other solid lubricants, the polymer material has the advantages that the frictional wear performance is not influenced by atmosphere, and the tribological characteristics of PTFE in vacuum are enough to explain the characteristic.
Self-lubricating composite materials are classified into two types, namely polymer-based composite materials and metal-based composite materials. PTFE is most commonly used for polymer-based composites. The metal-based composite material is developed on the basis of powder metallurgy, and proper lubricant powder is added into metal powder, and the metal powder is pressed and sintered into a blank, wherein the Ag-MoS is commonly used2-a graphitic ternary system material.
The working environment of the space lubricant is very complex, and the factors which have direct relation with the lubricating performance of the space lubricant mainly comprise high vacuum, extreme environment temperature, strong radiation, atomic oxygen and the like. The relevant data report that the space pressure of a spacecraft in operation on a high-orbit space load is 10-11Pa, the space pressure born by the track is 10 when the track runs on the near ground-5～10-7Range of Pa magnitude. Lubricants used in such special circumstances should not only have good tribological properties, but must also have ultra-low vapor pressure properties.
The side of the aircraft facing the sun in the universe bears the intense radiation of the sun, the surface temperature can reach 100-200 ℃, the side facing the sun is influenced by the extremely cold environment of the universe space, and the surface temperature can resist minus 100-minus 200 ℃. In space environment, various radiations such as cosmic rays, ultraviolet rays, X rays and the like exist, some lubricants lose lubricating property under long-term radiation, and the radiation resistance of the high polymer material is poor, but the lubricating property is 104Gy～105Gy also did not change. The main component in the atmosphere of the predetermined orbit of the space is atomic oxygen, the material is easily oxidized and damaged by the high-activity atomic oxygen, and most lubricants are damaged in the atomic oxygen for no more than 10 years at most.
The research work of the space lubrication technology in China is effective, and in the aspect of liquid lubrication, the chlorphenyl silicone oil with wide liquid temperature range, low volatility and better lubricating property is designed and synthesized; mineral oil-based and silicone oil-based greases and greases for space use have been developed. In the aspect of solid lubrication, the research on the preparation science and technology of multilayer metal coating materials and nano-structure composite coating materials is developed by combining the development trends of the compounding, the layering and the nano-compounding in the scientific and technical field of coating materials, and the influence rule of the composition and the distribution characteristics of the coating on the friction and wear performance of the coating is mainly studied. Meanwhile, expert scholars, in combination with related scientific and technical research results, have developed various polymer-based and metal-based self-lubricating materials, such as Polytetrafluoroethylene (PTFE) -based and polyimide-based bearing retainer materials, and the like.
Although China has accumulated for more than 60 years in the field of space tribology, particularly has made great progress in the field of space lubricating materials, and has obtained a lot of main research results, the difference still exists with the developed countries, and according to the national conditions of China, the research on solid lubricating materials and related technologies is still one of the key works of the space tribology research.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a space solid lubricant coating which is low in friction coefficient, small in abrasion loss, uniform and continuous in structure and about 20 mu m in thickness and a preparation method thereof. The method is scientific and reasonable, has great achievement transformation potential and wide practical value, and is mainly applied to spacecraft lubrication devices.
The purpose of the invention is realized by adopting the following technical scheme. A solid lubricant coating component PTFE particle is 40-100 meshes, the friction coefficient is low (0.125-0.185), the abrasion loss is small (0.3-4.8 g), the structure is uniform and continuous, and the thickness is about 20 mu m. Wherein in the step of testing the vacuum tribology performance, the vacuum degree in the vacuum chamber of the testing machine is about 10-2MPa-10-7MPa, load of 4N-12N, speed of 0.2m/s-2.4m/s, friction distance of 1000m, the material of the dual-surface is a standard bearing steel ball (GCr 15), the size is phi 10mm, and the hardness is HRC 66.6.
And (4) analyzing the mechanism of the vacuum tribological performance of the PTFE coating.
The tribological properties of PTFE coatings are influenced by a number of factors, mainly by the environment, load, speed, contact pattern, surface roughness, etc. Under the vacuum environment condition, the tribological performance of the PTFE coating is mainly influenced by load and speed, and factors such as environment, contact mode, surface roughness and the like do not change. In the initial stage of the whole friction process, the friction contact mode is point-surface type, the surface of the coating material has certain surface roughness, mainly abrasive wear, the furrow effect is realized, and the friction coefficient is rapidly increased in the initial stage of friction. As friction progresses, the PTFE enters plastic deformation, sticking, and material transfer states, resulting in an increasing coefficient of friction. The surface of the PTFE coating material forms a self-lubricating film that acts as a solid lubricant so that the two materials enter a stable friction phase earlier and the coefficient of friction no longer changes as the sliding distance increases. Therefore, the friction coefficient of the PTFE coating material in vacuum has basically consistent change trend along with speed and load.
The symmetrical structure of PTFE makes the molecular chain have high rigidity, and the abrasive dust accumulated on the friction surface is difficult to embed into the matrix again. At lower speeds, the abrasive dust enriched on the friction surface after wear of the coating material acts as a solid lubricant with increasing speed, which increases the effect of the lubricant and thus reduces the amount of wear.
In the initial stage of friction, because the surfaces of the two materials have certain surface roughness, the contact mode of the PTFE coating material and the GCr15 steel is point-surface, and a lubricating film is formed on the surface of the PTFE coating material in the friction process. Therefore, the amount of wear decreases with increasing speed. The contact mode is changed from point-surface type to surface-surface type along with the friction. Under the same wearing condition, along with the improvement of speed, the corresponding increase of shear force value that PTFE coating material surface received, the probability that the abrasive dust drops increases, the wear resistance of material descends, simultaneously, along with the increase of speed, the friction heat that PTFE coating material wearing surface gathered at the wearing and tearing in-process increases, PTFE coating material is by the glass transition state under the low temperature condition gradually to viscous flow state transition, the degree of softening that PTFE coating material performance increases gradually, the macromolecule activity of polymer PTFE base member increases, make the probability that "step" appearance on wear scar surface drops increase, the abrasive dust increases, the wearing and tearing volume also increases thereupon.
The influence of the load on the friction performance of the PTFE coating material is mainly reflected in that the PTFE coating material is a viscoelastic material, and the PTFE generates viscoelastic deformation under the action of external force.
On one hand, with the further increase of load, the friction heat generated in the abrasion process is increased, the viscoelasticity degree shown by the PTFE coating material is increased, the entanglement among polymer chains of the PTFE coating material is released strongly, the high polymer PTFE enters a viscous state, the whole polymer chains participate in movement, the surface is melted, and the activity of the polymer surface molecules is greatly increased. Meanwhile, as heat is generated by friction, the increase in temperature of the friction surface causes a decrease in crystallinity of the material around the wear scar, resulting in an increase in the amount of wear.
The heat of friction can evaporate the PTFE coating material, and the evaporation rate is 10 at 100 DEG C-9g/(cm2S), when the temperature rises to 350 ℃, the evaporation rate increases sharply to 10-4g/(cm2S) above. With the increase of the temperature, the capability of molecular motion is enhanced microscopically, and the deformability of the material is improved macroscopically, so that the material has good toughness. The enhancement of the molecular mobility can relieve the action of external force. From a tribological point of view, the wear of the PTFE coating material decreases under load, but above a certain temperature, the PTFE coating material changes rapidly from a hard, glassy state to a so-called "viscoelastic state" wear, which is both elastic and viscous.
On the other hand, along with the increase of the melting phenomenon at the grinding mark, the adhesion capability of the PTFE coating substrate to the grinding dust is reduced, the probability of the grinding dust entering the substrate is reduced continuously, and the abrasion loss in the friction process is increased.
The invention has the following advantages:
1. the solid lubricant has low friction coefficient and less abrasion loss;
2. the solid lubricant has the thickness of about 20 mu m, has uniform and continuous structure and is mainly applied to lubricating devices of spacecrafts;
3. the preparation method of the solid lubricant is scientific and reasonable, and has great achievement transformation potential and wide practical value.
Drawings
FIG. 1 is a topographical view of the coating;
FIG. 2 is a graph of coating coefficient of friction as a function of speed;
FIG. 3 is a graph of coating wear as a function of speed;
FIG. 4 is a graph of coating coefficient of friction as a function of load;
FIG. 5 is a graph of coating wear as a function of load;
FIG. 6 is a graph of the wear surface topography of the coating.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1: a space solid lubrication coating and a preparation method thereof, wherein the coating component of a solid lubricant is PTFE particles with the size of 40-100 meshes, and the preparation method mainly comprises the steps of sample preparation, polishing treatment, PTFE particle screening, coating deposition, surface wiping, vacuum tribology performance testing and abrasive dust collection;
polishing a LY12 sample, screening PTFE particles, depositing a coating, wiping the surface, testing the vacuum tribology performance and collecting abrasive dust, and then testing the vacuum tribology behavior; the specific process is as follows:
1. polishing treatment
Polishing the upper surface and the lower surface of a LY12 sample by using a polishing machine, wherein the size of the sample is phi 70mm multiplied by 10mm, and the polishing time is 2min, so that the surface of the sample is bright but no oxidation phenomenon occurs;
PTFE particle screening
Crushing PTFE particles by a crusher or manually to obtain PTFE particles with the size of about 60 meshes;
3. deposition coating
By means of magnetron sputteringSputtering deposition coating treatment is carried out on the upper surface and the lower surface of a LY12 sample by an emission instrument, a PTFE target with the substrate size of phi 70mm multiplied by 10mm and the purity of 99.999 percent is selected, and pressure intensity (0.6 Pa and 1.0 Pa), Ar and N are set2The flow ratio (10: 15 sccm), the substrate temperature (220 ℃), and the sputtering time of 60 min; when the experiment is started, the background vacuum degree is pumped to 4.0 x 10 by the mechanical pump-molecular pump system -5Pa, after the parameters are adjusted, opening a baffle plate and starting sputtering and coating; after sputtering is finished, closing the baffle, the radio frequency power supply, the heating device and the gas valve in sequence, and taking out a sample when the indicated temperature of the substrate is reduced to room temperature;
4. surface wiping
Carrying out surface wiping treatment on PTFE coatings on the upper surface and the lower surface of an LY12 sample by using an acetone solution, and removing surface deposits;
5. vacuum tribology Performance testing
Testing tribological performance of the coating by using ball-disk type (BYTT-1000) vacuum friction abrasion tester with vacuum degree of 1 × 10-5MPa, load of 6N, speed of 0.2m/s-2.4m/s, friction distance of 1000m, dual-surface material of standard bearing steel ball (GCr 15), size of phi 10mm, and hardness of HRC 66.6;
6. abrasive dust collection
Collecting PTFE coating abrasive dust by using paper dust and acetone solution for later use;
as shown in fig. 1, the PTFE coating structure is uniform, continuous, and has an average thickness of 20 μm;
as shown in fig. 2-3, the coefficient of friction of the PTFE coating increases and then decreases with increasing speed, and the amount of wear increases with increasing speed.
Example 2: a space solid lubrication coating and a preparation method thereof, wherein the coating component of a solid lubricant is PTFE particles with the size of 40-100 meshes, and the preparation method mainly comprises the steps of sample preparation, polishing treatment, PTFE particle screening, coating deposition, surface wiping, vacuum tribology performance testing and abrasive dust collection;
polishing a LY12 sample, screening PTFE particles, depositing a coating, wiping the surface, testing the vacuum tribology performance and collecting abrasive dust, and then testing the vacuum tribology behavior; the specific process is as follows:
1. polishing treatment
Polishing the upper surface and the lower surface of a LY12 sample by using a polishing machine, wherein the size of the sample is phi 70mm multiplied by 10mm, and the polishing time is 3min, so that the surface of the sample is bright but no oxidation phenomenon occurs;
PTFE particle screening
Crushing PTFE particles by a crusher or manually to obtain particles with the size of about 80 meshes;
3. deposition coating
Performing sputtering deposition coating treatment on the upper surface and the lower surface of a LY12 sample by using a magnetron sputtering instrument, selecting a PTFE target with the substrate size of phi 70mm multiplied by 10mm and the purity of 99.999%, and setting pressure (0.6 Pa and 1.0 Pa), Ar and N2The flow ratio (10: 15 sccm), the substrate temperature (220 ℃), and the sputtering time of 60 min; when the experiment is started, the background vacuum degree is pumped to 4.0 x 10 by the mechanical pump-molecular pump system -5Pa, after the parameters are adjusted, opening a baffle plate and starting sputtering and coating; after sputtering is finished, closing the baffle, the radio frequency power supply, the heating device and the gas valve in sequence, and taking out a sample when the indicated temperature of the substrate is reduced to room temperature;
4. surface wiping
Carrying out surface wiping treatment on PTFE coatings on the upper surface and the lower surface of an LY12 sample by using an acetone solution, and removing surface deposits;
5. vacuum tribology Performance testing
Testing tribological performance of the coating by using ball-disk type (BYTT-1000) vacuum friction abrasion tester with vacuum degree of 1 × 10-5MPa, load of 4N-12N, speed of 0.8m/s, friction distance of 1000m, dual-surface material of standard bearing steel ball (GCr 15), size of phi 10mm, and hardness of HRC 66.6;
6. abrasive dust collection
Collecting PTFE coating abrasive dust by using paper dust and acetone solution for later use;
as shown in fig. 4-5, the coefficient of friction of the PTFE coating decreases with increasing load, and the amount of wear does not change much with increasing load;
as shown in FIG. 6, the worn surface of the PTFE coating becomes smoother, a self-lubricating film is formed on the surface, and furrowing occurs.

Claims (2)

1. A spatial solid lubricating coating is characterized in that PTFE particles are used as a solid lubricant coating component, the size of the PTFE particles is 40-100 meshes, the solid lubricant coating is uniform and continuous, and the average thickness of the solid lubricant coating is 20 micrometers;
the space solid lubricating coating is prepared by the following method: the method comprises the steps of sample preparation, polishing treatment, PTFE particle screening, coating deposition and surface wiping;
(1) polishing treatment
Polishing the upper surface and the lower surface of the LY12 sample by a polishing machine, wherein the sample has the size of phi 70mm multiplied by 10mm, the polishing time is 2min, the surface of the sample is bright, and the oxidation phenomenon is avoided;
(2) PTFE particle screening
Crushing PTFE particles by a crusher or manually, wherein the size of the PTFE particles is 60 meshes;
(3) deposition coating
Performing sputtering deposition coating treatment on the upper surface and the lower surface of a LY12 sample by using a magnetron sputtering instrument, selecting a PTFE target with the substrate size of phi 70mm multiplied by 10mm and the purity of 99.999%, and setting the pressure to be 0.6Pa or 1.0Pa, Ar and N2 The flow ratio is 10:15sccm, the substrate temperature is 220 ℃, and the sputtering time is 60 min; when the experiment is started, the background vacuum degree is pumped to 4.0 x 10 by the mechanical pump-molecular pump system-5Pa, after the parameters are adjusted, opening a baffle plate and starting sputtering and coating; after sputtering is finished, closing the baffle, the radio frequency power supply, the heating device and the gas valve in sequence, and taking out a sample when the indicated temperature of the substrate is reduced to room temperature;
(4) surface wiping
Carrying out surface wiping treatment on PTFE coatings on the upper surface and the lower surface of an LY12 sample by using an acetone solution, and removing surface deposits;
the service vacuum degree of the space solid lubricating coating is 1 multiplied by 10-5MPa, load of 6N, speed of 0.2-2.4 m/s, friction distance of 1000m, standard bearing steel ball GCr15 as dual-surface material,the size is phi 10mm, and the hardness is HRC 66.6.
2. A spatial solid lubricating coating is characterized in that PTFE particles are used as a solid lubricant coating component, the size of the PTFE particles is 40-100 meshes, the solid lubricant coating is uniform and continuous, and the average thickness of the solid lubricant coating is 20 micrometers;
the space solid lubricating coating is prepared by the following method: the method comprises the steps of sample preparation, polishing treatment, PTFE particle screening, coating deposition and surface wiping;
(1) polishing treatment
Polishing the upper surface and the lower surface of the LY12 sample by a polishing machine, wherein the sample has the size of phi 70mm multiplied by 10mm, the polishing time is 3min, the surface of the sample is bright, and the oxidation phenomenon is avoided;
(2) PTFE particle screening
Crushing PTFE particles by a crusher or manually, wherein the size of the PTFE particles is 80 meshes;
(3) deposition coating
Performing sputtering deposition coating treatment on the upper surface and the lower surface of a LY12 sample by using a magnetron sputtering instrument, selecting a PTFE target with the substrate size of phi 70mm multiplied by 10mm and the purity of 99.999%, and setting the pressure to be 0.6Pa or 1.0Pa, Ar and N2 The flow ratio is 10:15sccm, the substrate temperature is 220 ℃, and the sputtering time is 60 min; when the experiment is started, the background vacuum degree is pumped to 4.0 x 10 by the mechanical pump-molecular pump system-5Pa, after the parameters are adjusted, opening a baffle plate and starting sputtering and coating; after sputtering is finished, closing the baffle, the radio frequency power supply, the heating device and the gas valve in sequence, and taking out a sample when the indicated temperature of the substrate is reduced to room temperature;
(4) surface wiping
Carrying out surface wiping treatment on PTFE coatings on the upper surface and the lower surface of an LY12 sample by using an acetone solution, and removing surface deposits;
the service vacuum degree of the space solid lubricating coating is 1 multiplied by 10-5MPa, load of 4-12N, speed of 0.8m/s, friction distance of 1000m, dual-surface material of standard bearing steel ball GCr15, size of phi 10mm, and hardness of HRC 66.6.
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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN103898444A (en) * 2012-12-27 2014-07-02 深圳富泰宏精密工业有限公司 Coating member and preparation method thereof
CN204097554U (en) * 2014-08-20 2015-01-14 上海航天设备制造总厂 The corrosion-resistant solid lubricant film of polytetrafluoroethylene (PTFE) base

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Publication number Priority date Publication date Assignee Title
KR100391307B1 (en) * 2001-06-04 2003-07-16 한라공조주식회사 Method for preparing a solid film lubricant

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Publication number Priority date Publication date Assignee Title
CN103898444A (en) * 2012-12-27 2014-07-02 深圳富泰宏精密工业有限公司 Coating member and preparation method thereof
CN204097554U (en) * 2014-08-20 2015-01-14 上海航天设备制造总厂 The corrosion-resistant solid lubricant film of polytetrafluoroethylene (PTFE) base

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