CN116334564A - Method for lubricating surface and self-catalytic composite carbon-based film solid-liquid composite lubricating system - Google Patents
Method for lubricating surface and self-catalytic composite carbon-based film solid-liquid composite lubricating system Download PDFInfo
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- CN116334564A CN116334564A CN202310523838.8A CN202310523838A CN116334564A CN 116334564 A CN116334564 A CN 116334564A CN 202310523838 A CN202310523838 A CN 202310523838A CN 116334564 A CN116334564 A CN 116334564A
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Images
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
- B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
- B05C3/09—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles
- B05C3/10—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles the articles being moved through the liquid or other fluent material
-
- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
- C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
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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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/16—Paraffin waxes; Petrolatum, e.g. slack wax
- C10M2205/163—Paraffin waxes; Petrolatum, e.g. slack wax used as base material
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/16—Naphthenic acids
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
- C10M2207/2835—Esters of polyhydroxy compounds used as base material
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- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a method for lubricating a surface and an autocatalysis composite carbon-based film solid-liquid composite lubricating system, which relate to the technical field of material surface modification and consist of a multi-element doped DLC nano composite film and composite lubricating liquid, wherein the multi-element doped DLC nano composite film is positioned on the surface of a titanium alloy substrate; the multi-element dopant in the multi-element doped DLC nano-composite film comprises metal oxide; the metal in the metal oxide is at least selected from Ti; the composite lubricating fluid comprises base oil and a phosphorus-free additive; the above-mentioned phosphorus-free additive is selected from at least one of naphthenic acid and naphthenic alcohol. The composite lubrication system prepared by the invention has lower friction coefficient and improved wear resistance; the titanium alloy composite material has better mechanical property, enhanced film hardness, further increased bonding capability with a substrate and high application value, and is expected to be a novel technology for solving the problem of solid-liquid lubrication integration of high-performance titanium alloy engine parts.
Description
Technical Field
The invention belongs to the technical field of material surface modification, and particularly relates to a method for lubricating a surface and an autocatalytic composite carbon-based film solid-liquid composite lubricating system.
Background
The engine is an important way for energy conservation and emission reduction of automobiles, and the titanium alloy becomes a high-quality potential manufacturing material for the light weight of automobile engine parts according to the lower density and excellent mechanical property of the titanium alloy, but the poor friction lubricating property of the titanium alloy greatly limits the wide application of the titanium alloy in production practice.
Diamond-like carbon (DLC) films have many excellent properties such as high hardness, low coefficient of friction, high wear resistance, and good chemical stability, thermal conductivity, etc. DLC as a novel functional thin film material in many fields such as: the method has great application prospect in fields such as tribology, vacuum microelectronics, optoelectronics, aerospace, biomedical materials, M/NEMS and the like. The low friction coefficient of the DLC film can effectively reduce friction loss of key parts of an engine, and is the focus of research in the field of energy conservation and emission reduction of the engine internationally at present. However, lubricating oil antifriction agents, antiwear agents and extreme pressure agents widely used in these fields are designed and synthesized based on the surface reaction with metal materials, and elements such as sulfur, phosphorus, chlorine and the like which are unfavorable for environmental protection are widely utilized. The chemical stability of the DLC surface causes that the DLC surface is not easy to form effective antifriction and antiwear effects with the additives, wherein the extreme pressure antiwear agent ZDDP and the antifriction agent MODTC which are most successfully and widely applied not only contain elements such as sulfur, phosphorus and the like, but also have difficult formation of a friction film with an antiwear effect on the DLC surface due to the chemical inertness of the DLC, and the friction coefficient is generally higher.
Disclosure of Invention
The invention aims to provide a method for lubricating a surface and an autocatalytic composite carbon-based film solid-liquid composite lubricating system, wherein the composite lubricating system has a lower friction coefficient and improved wear resistance; and the coating has better mechanical property, the hardness of the film layer is enhanced, the bonding capability with the substrate is further improved, and the application value is high.
The technical scheme adopted by the invention for achieving the purpose is as follows:
an oxide composite carbon-based film solid-liquid composite lubrication system with an autocatalysis effect comprises a multi-element doped DLC nano composite film and composite lubrication liquid which are positioned on the surface of a substrate;
the multi-element dopant in the multi-element doped DLC nano-composite film comprises metal oxide; the metal in the metal oxide is at least selected from Ti;
the composite lubricating fluid comprises base oil and a phosphorus-free additive; the above-mentioned phosphorus-free additive is selected from at least one of naphthenic acid and naphthenic alcohol. The invention adopts the magnetron sputtering technology to deposit the carbon-based film compounded with different oxides on the surface of the titanium alloy, has better mechanical property, enhances the hardness of the film layer, obviously reduces the internal stress, promotes the bonding force with the substrate and shows better interface bonding capability. Meanwhile, the novel solid-liquid composite lubricating system is constructed together with PAO, polyol ester lubricating oil and sulfur-and phosphorus-free environment-friendly additives such as alcohol, polybasic cyclic acid and the like, so that the novel solid-liquid composite lubricating system has more excellent friction performance, obviously reduced friction coefficient, better wear resistance and obviously reduced wear rate. In addition, the composite lubricating system constructed by the invention can reconstruct additives such as lubricating base oil or polybasic cyclic acid and polybasic cyclic alcohol into carbon-based compounds in the friction and abrasion process by utilizing the catalytic effect of oxides, and the carbon-based compounds are deposited at the abrasion positions of the coating to self-repair the abrasion-based compounds, so that the long-acting wear-resistant lubricating effect is achieved.
Specifically, the base material includes a titanium alloy.
Specifically, the metal in the metal oxide further includes one of Ce, la, al, fe and Bi.
Specifically, the base oil is at least one selected from the group consisting of PAO oil, liquid paraffin and polyol ester.
Specifically, the PAO oil is selected from one of PAO4, PAO6 and PAO 8.
Specifically, the naphthenic acid includes at least one of cyclopropanecarboxylic acid, cyclobutanecarboxylic acid, cyclopentanecarboxylic acid, or cyclopropanedicarboxylic acid.
Specifically, the cycloalkanol includes at least one of cyclopropyl alcohol, cyclobutyl alcohol, cyclopentyl alcohol, or dihydroxycyclopropyl alcohol.
Further, the non-phosphorus additive also comprises an ionic liquid.
Specifically, the anion of the ionic liquid is BF 4 - The cation is alkyl imidazole ring.
Further, the composite lubricating fluid also comprises Cu nano particles.
The invention also discloses a method for lubricating a surface, comprising the following steps: forming an autocatalytic composite carbon-based film solid-liquid composite lubrication system on the surface of the substrate material.
The self-catalytic composite carbon-based film solid-liquid composite lubrication system comprises the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect.
The invention also discloses a preparation method of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect, which comprises the following steps:
(1) Preparing an oxide composite carbon-based film, and treating the surface of the titanium alloy by adopting a magnetron sputtering technology to obtain the titanium alloy;
(2) The preparation of the solid-liquid composite lubrication system of the oxide composite carbon-based film is realized by compounding the oxide composite carbon-based film and the composite lubrication liquid by adopting a dipping-lifting method.
Further specifically, the preparation method of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect comprises the following steps:
(1) Preparing an oxide composite carbon-based film (DLC), and treating the surface of the titanium alloy by adopting a reaction magnetron sputtering technology, wherein the preparation method specifically comprises the following steps:
before deposition, sequentially ultrasonic treating the titanium alloy substrate in absolute ethyl alcohol and acetone for 10-15 min, taking out, naturally airing, then placing in a vacuum chamber, and pumping the vacuum chamber to 1-3X 10 -3 Pa, filling Ar, and cleaning and activating for 10-20 min under the conditions of air flow of 100-120 sccm, vacuum degree of 1-1.2 Pa and 800-1000V (duty ratio is 10-20 percent); the film deposition takes a graphite target (sputtering current is 3-5A) and a composite metal target (sputtering current is 1-4A) as sputtering targets, the bias voltage of a fixed substrate is 500V (duty ratio is 50-60%), the target base distance is 80-100 mm, the total air pressure in a cavity is 0.8-1 Pa, and the total sputtering duration is 80-100 min; intracavity O 2 The flow ratio of Ar is 15-25:40, and the flow rate of Ar is 120-140 sccm; after the deposition is finished, closing the equipment, cooling for 1-2 hours, and taking out; the thickness of the oxide composite carbon-based film is 0.5-4 mu m;
(2) The preparation of the oxide composite carbon-based film solid-liquid composite lubrication system adopts an immersion-lifting method to compound the oxide composite carbon-based film with composite lubrication liquid, and specifically comprises the following steps:
preparation of a composite lubricating liquid: adding a phosphorus-free additive into base oil, mechanically stirring uniformly, and performing ultrasonic treatment for 30-40 min under the power of 500-600W to obtain a composite lubricating liquid;
and (3) immersing the oxide composite carbon-based film obtained in the step (1) in a composite lubricating liquid, wherein the immersing time is controlled to be 2-6 min, and the lifting speed is controlled to be 20-40 mm/s, so as to obtain the solid-liquid composite lubricating system of the oxide composite carbon-based film.
Specifically, the thickness of the oxide composite carbon-based film is 0.5-4 [ mu ] m.
Specifically, in the preparation process of the composite lubricating liquid, the addition amount of the phosphorus-free additive is 1.5-2.5wt%.
Specifically, the oxide content of the oxide composite carbon-based film is 0.1-30wt%.
Specifically, the preparation method of the composite lubricating fluid further comprises the following steps: and adding the Cu nano particles into the base oil at the concentration of 0.1-1wt%, adding the phosphorus-free additive, mechanically stirring uniformly, and performing ultrasonic treatment for 30-40 min under the power of 500-600W to obtain the composite lubricating liquid.
Further preferably, the phosphorus-free additive comprises modified oleic acid; wherein the modified oleic acid is obtained by esterifying lactic acid leaf alcohol ester to obtain oleic acid. The modified oleic acid prepared by modifying oleic acid with lactic acid leaf alcohol ester is used as an additive in a composite lubricating liquid, and the prepared oxide composite carbon-based film solid-liquid composite lubricating system has more excellent friction performance, further reduces friction coefficient and wear rate, improves film hardness, further reduces internal stress and improves mechanical performance of the composite lubricating system. The reason is probably that the modified oleic acid prepared by modifying oleic acid with lactic acid leaf alcohol ester introduces more polar functional groups in the structure, which is helpful for increasing the solubility of lubricating oil additives; the modified oleic acid can better adsorb the surface of the DLC composite film, and the abrasion resistance of the DLC composite film can be improved by inhibiting graphitization of the film in the friction process; in addition, the friction pair can be compounded with Cu nano particles, so that the dispersing capability of the friction pair is further improved, the micro-bearing effect of the Cu nano particles is better exerted, a physical adsorption layer is formed on the surface of the friction pair, a sliding friction layer is formed on the friction pair in the friction process, and a rolling friction layer which is not in direct contact is formed between the friction pairs, so that a better antifriction and antiwear effect is further shown.
The invention also discloses a preparation method of the modified oleic acid, which comprises the following steps: under the condition of a catalyst, the lactic acid leaf alcohol ester and oleic acid undergo an esterification reaction to prepare the modified oleic acid.
Further specifically, the preparation method of the modified oleic acid comprises the following steps:
mixing oleic acid and lactic acid leaf alcohol ester, adding toluene and catalyst ZnF 2 Then reacting for 6-8 hours under the protection of nitrogen at 160-170 ℃; cooling, vacuum filtering until the filtrate is clear and transparent, drying with anhydrous magnesium sulfate, vacuum distilling to remove solvent, and separating and purifying by column chromatography to obtain modified oleic acid.
Specifically, the molar ratio of oleic acid to lactic acid leaf alcohol ester is 1-1.5:1; the solid-to-liquid ratio of oleic acid to toluene is 0.5-1 g/1 mL; catalyst ZnF 2 The using amount of the catalyst is 6-9wt% of oleic acid.
Still another object of the present invention is to provide a use of the above-mentioned oxide composite carbon-based thin film solid-liquid composite lubrication system having an autocatalytic effect for enhancing friction lubrication performance of parts for an engine.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a metal oxide composite carbon-based film solid-liquid composite lubrication system with an autocatalysis effect is constructed on the surface of the titanium alloy, wherein the DLC coating has better mechanical properties, the hardness of the film layer is enhanced, the internal stress is obviously reduced, and the binding force with a substrate is improved; meanwhile, the composite system has more excellent friction performance, the friction coefficient is obviously reduced, and the composite system has better wear resistance and obviously reduced wear rate; meanwhile, naphthenic acid or naphthenic alcohol is adopted as an additive to be applied to the composite lubricating liquid, and the carbon-based compound can be generated in situ through the friction catalysis effect, so that the self-repairing effect can be formed, the friction performance of the oxide composite carbon-based film solid-liquid composite lubricating system is further improved, the friction coefficient and the wear rate are further reduced, and the service life is further prolonged. The metal oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect, which is constructed by the invention, realizes the effects of efficient lubrication and in-situ self-repair in a contact area through the friction catalysis effect, and is expected to provide a new thought for realizing the solid-liquid lubrication integrated modification technology of key high-performance engine parts by new energy-saving and emission-reduction standards.
Therefore, the invention provides a method for lubricating the surface and an autocatalytic composite carbon-based film solid-liquid composite lubricating system, wherein the composite lubricating system has lower friction coefficient and improved wear resistance; and the coating has better mechanical property, the hardness of the film layer is enhanced, the bonding capability with the substrate is further improved, and the application value is high.
Drawings
FIG. 1 is a schematic structural view of an oxide composite carbon-based thin film according to example 1 of the present invention;
FIG. 2 is a Raman profile and Raman spectrum of the dual ball contact region of the coatings prepared in examples 1 and 5 of the present invention;
FIG. 3 is a diagram of TiO according to the invention 2 The morphology of a coating abrasion mark area and a Raman spectrum;
FIG. 4 is an infrared spectrum of modified oleic acid and its oleic acid prepared in example 12 of the invention;
FIG. 5 is an SEM image of an oxide composite carbon-based thin film prepared in example 6 of the present invention;
FIG. 6 is an SEM image of an oxide composite carbon-based thin film prepared in comparative example 1 of the present invention;
FIG. 7 shows the results of the friction coefficient and wear rate tests of the composite lubrication systems prepared in examples 1 to 5 and comparative example 1;
FIG. 8 shows the results of the friction coefficient and wear rate tests of the composite lubrication systems prepared in examples 6 to 12 of the present invention.
Reference numerals:
1-oxide composite carbon-based thin film layer (DLC), 2-titanium alloy substrate, 3-oxide.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the following describes in detail various embodiments of the present invention with reference to the embodiments. However, those of ordinary skill in the art will understand that in various embodiments of the present invention, numerous technical details have been set forth in order to provide a better understanding of the present application. However, the technical solutions claimed in the present application can be implemented without these technical details and with various changes and modifications based on the following embodiments.
The metal targets used in the embodiment of the invention are all commercially available. Wherein the weight part ratio of La to Ce in the La-Ce alloy target is 1:2, and the weight part ratio of La to Ti in the La-Ti alloy target is 1:3; the weight ratio of La to Al of the La-Al alloy target is 1:4.
The PAO oil used in the embodiment of the invention is PAO6.
Example 1:
preparation of an oxide composite carbon-based film solid-liquid composite lubrication system with an autocatalysis effect:
(1) The preparation of the oxide composite carbon-based film (DLC) adopts a reaction magnetron sputtering technology to treat the surface of the titanium alloy, and the structural schematic diagram is shown in figure 1, and specifically comprises the following steps:
before deposition, the titanium alloy (Ti 6 Al 4 V) sequentially ultrasonic treating the substrate in absolute ethanol and acetone for 10min, taking out, naturally airing, placing in a vacuum chamber, and pumping the vacuum chamber to 3×10 air pressure -3 Pa, filling Ar, cleaning and activating for 15min under the conditions of 120sccm of air flow and 1Pa of vacuum degree and 1000V (duty ratio is 10 percent); the film deposition takes a graphite target (sputtering current is 5A) and a Ti metal target (sputtering current is 2.5A) as sputtering targets, the bias voltage of a fixed substrate is 500V (duty ratio is 50%), the base distance of the targets is 100mm, the total air pressure in a cavity is 0.8Pa, and the total sputtering duration is 100min; intracavity O 2 Ar flow ratio is 20:40, ar flow is 130sccm; after the deposition is finished, the equipment is closed, and the equipment is taken out after being cooled for 2 hours; the thickness of the oxide composite carbon-based film is 2.3 mu m; the oxide content of the oxide composite carbon-based film is 16.8wt%;
(2) The preparation of the oxide composite carbon-based film solid-liquid composite lubrication system adopts an immersion-lifting method to compound the oxide composite carbon-based film with composite lubrication liquid, and specifically comprises the following steps:
the compound lubricating fluid in the embodiment is PAO6 lubricating oil;
immersing the oxide composite carbon-based film obtained in the step (1) in a composite lubricating liquid, controlling the immersion time to be 5min and the lifting speed to be 36mm/s, and obtaining the solid-liquid composite lubricating system of the oxide composite carbon-based film.
Example 2:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of the embodiment 1 in that:
in the preparation process of the oxide composite carbon-based film in the step (1), the target is a La metal target, and the sputtering current is 1.5A.
Example 3:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of the embodiment 1 in that:
in the preparation process of the oxide composite carbon-based film in the step (1), the target is a Ce metal target, and the sputtering current is 3A.
Example 4:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of the embodiment 1 in that:
in the preparation process of the oxide composite carbon-based film in the step (1), the target is an Al metal target, and the sputtering current is 2A.
Example 5:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of the embodiment 1 in that:
adding additive naphthenic acid, specifically cyclopropane carboxylic acid, into the composite lubricating liquid in the step (2), adding cyclopropane carboxylic acid (the addition amount is 2 wt%) into PAO oil, mechanically stirring uniformly, and performing ultrasonic treatment for 30min under 600W power to obtain the composite lubricating liquid.
Example 6:
preparation of an oxide composite carbon-based film solid-liquid composite lubrication system with an autocatalysis effect:
(1) Preparing an oxide composite carbon-based film (DLC), and treating the surface of the titanium alloy by adopting a reaction magnetron sputtering technology, wherein the preparation method specifically comprises the following steps:
before deposition, the titanium alloy (Ti 6 Al 4 V) sequentially ultrasonic treating the substrate in absolute ethanol and acetone for 10min, and taking out naturallyAir drying, and placing in a vacuum chamber, and pumping air pressure in the vacuum chamber to 3×10 -3 Pa, filling Ar, cleaning and activating for 15min under the conditions of 120sccm of air flow and 1Pa of vacuum degree and 1000V (duty ratio is 10 percent); the film deposition takes a graphite target (sputtering current is 5A) and a La-Ce alloy target (sputtering current is 2.5A) as sputtering targets, the bias voltage of a fixed substrate is 500V (duty ratio is 50%), the base distance of the targets is 100mm, the total air pressure in a cavity is 0.8Pa, and the total sputtering duration is 100min; intracavity O 2 Ar flow ratio is 20:40, ar flow is 130sccm; after the deposition is finished, the equipment is closed, and the equipment is taken out after being cooled for 2 hours; the thickness of the oxide composite carbon-based film is 2.3 mu m;
(2) The preparation of the oxide composite carbon-based film solid-liquid composite lubrication system adopts an immersion-lifting method to compound the oxide composite carbon-based film with composite lubrication liquid, and specifically comprises the following steps:
preparation of a composite lubricating liquid: naphthenic acid (cyclopropane dicarboxylic acid with the addition amount of 2 wt%) is added into PAO oil, and the mixture is mechanically stirred uniformly, and the mixture is subjected to ultrasonic treatment for 30min under the power of 600W to obtain a composite lubricating liquid;
immersing the oxide composite carbon-based film obtained in the step (1) in a composite lubricating liquid, controlling the immersion time to be 5min and the lifting speed to be 36mm/s, and obtaining the solid-liquid composite lubricating system of the oxide composite carbon-based film.
Example 7:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of example 6 in that:
in the preparation process of the oxide composite carbon-based film in the step (1), the target is La target, and the sputtering current is 1.5A.
Example 8:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of example 6 in that:
in the preparation process of the oxide composite carbon-based film in the step (1), the target is La-Ti alloy target, and the sputtering current is 3A.
Example 9:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of example 6 in that:
in the preparation process of the oxide composite carbon-based film in the step (1), the target is La-Al alloy target, and the sputtering current is 2A.
Example 10:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of example 6 in that:
in the composite lubricating liquid in the step (2), the additive is an ionic liquid, specifically 1-dodecyl-3-methylimidazole tetrafluoroborate.
Example 11:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of example 6 in that:
the preparation of the composite lubricating liquid in the step (2) comprises the following specific steps: the Cu nano particles are added into PAO oil at the concentration of 0.6wt percent, oleic acid (the addition amount is 2wt percent) is added, and the mixture is mechanically stirred uniformly, and the ultrasonic treatment is carried out for 30 minutes under the power of 600W to obtain the composite lubricating liquid.
Example 12:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of example 11 in that:
in the composite lubricating liquid in the step (2), the modified oleic acid with the same molar weight is adopted to replace oleic acid.
Preparation of the modified oleic acid:
mixing oleic acid and lactic acid leaf alcohol ester according to the mol ratio of 1.3:1, adding toluene (the solid-to-liquid ratio of oleic acid to toluene is 0.8g:1 mL) and catalyst ZnF 2 (the use amount is 7.8wt% of oleic acid), and then reacting for 7 hours under the protection of nitrogen at 170 ℃; cooling, vacuum filtering until the filtrate is clear and transparent, drying with anhydrous magnesium sulfate, vacuum distilling to remove solvent, and separating and purifying by column chromatography (eluent ethyl acetate: petroleum ether=1:9, v/v) to obtain modified oleic acid.
Comparative example 1:
the preparation of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect is different from that of the embodiment 1 in that:
in the preparation process of the oxide composite carbon-based film in the step (1), a metal target is not used.
Test example 1:
raman characterization
Carrying out grinding mark area analysis by adopting a Raman spectrometer, wherein the laser wavelength is 532nm, and the wavelength range is 400-4000 cm -1 。
The contact area of the dual ball after friction of the coating prepared in example 1 was tested as described above and the results are shown in fig. 2. From the analysis in the figure, under different test conditions, the contact areas of the dual balls in the example 1 and the example 5 generate obvious Raman peaks at 1400-1600, and compared with the Raman peaks of DLC, the product is mainly a carbon-based product similar to DLC, and the product can promote the improvement of the tribological performance of a composite system. In example 5, the raman peak intensity is obviously stronger than that of example 1 due to the addition of cyclopropanecarboxylic acid, so that the addition of cyclopropanecarboxylic acid is beneficial to further improving the tribology of the composite lubrication system.
In addition, only TiO is selected 2 The coating was subjected to the same tribological tests as described above with the PAO6 base oil and raman characterization of the contact zone was performed. As shown in FIG. 3, it is found from the analysis of the graph that in the friction contact region, at 1356 and 1356 cm -1 And 1575cm -1 The obvious Raman peak is the characteristic peak of the carbon-based material, while the TiO is reserved outside the friction contact area 2 Raman characteristic peaks of (a) to account for TiO 2 Has the ability to catalyze the formation of carbon-based lubricating materials from PAO oils.
Characterization of infrared properties
The resolution is 4cm by using a Fourier infrared spectrometer -1 Wavelength range 500-4000 cm -1 。
The modified oleic acid prepared in example 12 and oleic acid were subjected to the above test, and the results are shown in fig. 4. From the analysis in the figure, it is found that the carbonyl peak position in the modified infrared spectrum prepared in example 12 is 1707cm compared with the infrared test result of oleic acid -1 Move to 1730cm -1 The conversion of the carboxycarbonyl group to an ester carbonyl group is illustrated, indicating successful production of the modified oleic acid in example 12.
SEM characterization
The test is carried out by adopting a thermal field type field emission scanning electron microscope and an energy spectrum component thereof, and the appearance of the film is observed.
The above-described test was performed on the oxide composite carbon-based thin films prepared in example 6 and comparative example 1, and the results are shown in fig. 5 to 6. From the analysis of the figure, it is understood that, in the SEM image of the oxide composite carbon-based thin film prepared in example 6, the surface of the thin film is relatively smoother and flatter, and the particle size and the number of agglomerated particles are significantly reduced, compared to the SEM image of the oxide composite carbon-based thin film prepared in comparative example 1.
Test example 2:
friction performance measurement
The experiment was performed using a micro-vibration friction wear tester. The experimental test process adopts a ball-disc reciprocating mode, and specific experimental conditions comprise: the rotation radius is 5mm, the rotation speed is 25, 50 and 200mm/s, the pressure is 10, 15 and 20N, the temperature is 25 ℃, and the test time is 30min; the friction pair above is a steel ball with the diameter of 6mm, the hardness of 58-52HRC, the elastic modulus of 208GPa and the Poisson's ratio of 0.3, and the material is Gcr 15. And (3) cleaning residual oil by using acetone after the friction test is finished, and observing the morphology of a friction interface by using a scanning electron microscope. The calculation formula of the wear rate of the friction pair under a lubrication system is as follows:
K=V/(FS)
wherein V represents the wear volume of the wear scar, mm 3 The method comprises the steps of carrying out a first treatment on the surface of the F represents the load during friction and N; s represents the friction full stroke, m.
The above test was performed on the composite lubrication systems prepared in examples 1 to 5 and comparative example 1, and the results are shown in fig. 7. From the analysis of the graph, the friction coefficient and the wear rate of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect prepared in the example 1 are obviously lower than those of the example 2 and the comparative example 1, and the effect of the example 2 is obviously better than that of the comparative example 1, so that the DLC film layer prepared by adopting Ti or La doping to prepare the metal oxide composite DLC film layer shows better friction performance, the friction coefficient is obviously reduced, the wear rate is reduced, and the friction and wear resistance is improved. Examples 3-4 have better effects than example 2 and comparative example 1, indicating that the use of Ce or Al doping to prepare the metal oxide composite DLC film layer can also further improve the friction performance of the composite lubrication system. The effect of example 5 is obviously better than that of example 1, and shows that the cyclopropanecarboxylic acid is used as an additive in the composite lubricating liquid, so that the friction performance of a composite lubricating system can be further enhanced, and the friction coefficient and the wear rate are further reduced.
The above test was performed on the composite lubrication systems prepared in examples 6 to 12, and the results are shown in fig. 8. From the analysis of the figure, the friction coefficient and the wear rate of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect prepared in example 6 are obviously lower than those of the oxide composite carbon-based film solid-liquid composite lubrication system prepared in example 7 and comparative example 1, and the effect of example 7 is obviously better than that of comparative example 1, so that the DLC film layer prepared by doping La and/or Ce shows better friction performance, the friction coefficient is obviously reduced, the wear rate is reduced, and the friction and wear resistance is improved. Examples 8-9 have better effects than example 7 and comparative example 1, indicating that the friction performance of the composite lubrication system can be further improved by preparing a metal oxide composite DLC film layer by doping La composite Ti or Al. The effect of example 12 is obviously better than that of example 11, and shows that the modified oleic acid prepared by modifying oleic acid with lactic acid leaf alcohol ester can be used as an additive in the composite lubricating liquid, so that the friction performance of the composite lubricating system can be further enhanced, and the friction coefficient and the wear rate are further reduced.
Test example 3:
hardness measurement
The test is carried out by using a Vickers microhardness tester nanoindentation instrument, the loading load is 10mN, and the holding time is 15s.
Film internal stress measurement
The test adopts a substrate deformation method, the curvature radius of the front surface and the rear surface of the substrate coating film is measured, and then the Stoney formula is adopted to calculate the internal stress of the film.
Film binding force measurement
The test was performed using a WS-2005 automatic scratch tester with a Rockwell diamond standard 120 cone angle indenter, R=0.2 mm. And obtaining the critical load of the film by using a scratch instrument in the experimental process. When the pressure head breaks the film, the film emits weak acoustic emission signals due to breakage or peeling, and the acoustic emission detection sensor detects the signals and then jumps; or observing the change of the friction coefficient, and when the friction coefficient suddenly rises, the applied load is the critical load of the film, namely the film base bonding strength.
The above test was performed on the composite lubrication systems prepared in examples 1 to 5 and comparative example 1, and the results are shown in table 1:
TABLE 1 results of physical and chemical film index test
| Sample of | Hardness (GPa) | Internal stress (GPa) | Film base binding force (N) |
| Example 1 | 22.8 | 1.46 | 25.6 |
| Example 2 | 21.1 | 1.75 | 20.1 |
| Example 3 | 22.4 | 1.64 | 22.3 |
| Example 4 | 20.6 | 1.31 | 23.1 |
| Example 5 | 22.3 | 1.43 | 25.9 |
| Comparative example 1 | 25.1 | 2.53 | 17.4 |
From the analysis in table 1, the internal stress of the oxide composite carbon-based thin film solid-liquid composite lubrication system with the self-catalytic effect prepared in example 1 is obviously smaller than that of example 2 and comparative example 1, and the film-based binding force is obviously higher than that of example 2 and comparative example 1; the effect of example 2 is also significantly better than that of comparative example 1, indicating that the preparation of metal oxide composite DLC film layers using Ti and La doping shows low internal stress and significantly enhanced bonding ability to the substrate. The effects of examples 3-4 are better than those of example 2 and comparative example 1, which shows that the preparation of the metal oxide composite DLC film layer by Ce or Al doping can further improve the internal stress of the composite lubrication system, enhance the bonding performance with the substrate, and improve the mechanical energy of the coating. Example 5 is significantly better than example 1, indicating that the use of naphthenic acid as an additive in a composite lubricating fluid can further improve the mechanical properties of the composite system.
The above test was performed on the composite lubrication systems prepared in examples 6 to 12, and the results are shown in table 2:
TABLE 2 results of physical and chemical film index test
| Sample of | Hardness (GPa) | Internal stress (GPa) | Film base binding force (N) |
| Example 6 | 23.8 | 1.26 | 28.6 |
| Example 7 | 22.1 | 1.45 | 25.4 |
| Example 8 | 23.4 | 1.14 | 27.3 |
| Example 9 | 22.6 | 1.31 | 27.1 |
| Example 10 | 22.9 | 1.10 | 28.5 |
| Example 11 | 23.2 | 1.17 | 29.0 |
| Example 12 | 25.5 | 0.89 | 29.2 |
From the analysis in table 2, the internal stress of the oxide composite carbon-based thin film solid-liquid composite lubrication system with the self-catalytic effect prepared in example 6 is obviously smaller than that of example 7 and comparative example 1, the film-based binding force is obviously higher than that of example 7 and comparative example 1, and the effect of example 2 is obviously better than that of comparative example 1, which shows that the DLC film layer prepared by doping La and/or Ce is better in hardness and the binding capability with the substrate is obviously enhanced. The effect of examples 8-9 is better than that of example 7 and comparative example 1, which shows that the preparation of the metal oxide composite DLC film layer by doping La composite Ti or Al can further improve the hardness of the composite lubrication system and enhance the bonding performance with the substrate. The hardness of the oxide composite carbon-based film solid-liquid composite lubrication system with the self-catalytic effect prepared in the example 12 is obviously better than that of the example 11, and the internal stress is obviously lower than that of the example 11, which shows that the modified oleic acid prepared by modifying oleic acid with lactic acid leaf alcohol ester is used as an additive in the composite lubrication liquid, so that the hardness of the composite lubrication system can be further enhanced, the internal stress of the system is reduced, and the mechanical property of the system is better improved.
The conventional technology in the above embodiments is known to those skilled in the art, and thus is not described in detail herein.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. An autocatalytic composite carbon-based film solid-liquid composite lubrication system is characterized in that: the nano-composite film comprises a multi-element doped DLC nano-composite film and a composite lubricating liquid which are positioned on the surface of a substrate;
the multi-element dopant in the multi-element doped DLC nano-composite film comprises metal oxide; the metal in the metal oxide is at least selected from Ti;
the composite lubricating fluid comprises base oil and a phosphorus-free additive; the phosphorus-free additive is selected from at least one of naphthenic acid and naphthenic alcohol.
2. The self-catalyzed composite carbon-based thin film solid liquid composite lubrication system of claim 1, wherein the metal of the metal oxide further comprises at least one of Ce, la, al, fe and Bi.
3. The self-catalyzed composite carbon-based thin film solid liquid composite lubrication system of claim 1, wherein the base oil is selected from at least one of PAO oil, liquid paraffin and polyol ester.
4. The self-catalyzed composite carbon-based thin film solid liquid composite lubrication system of claim 1, wherein the naphthenic acid comprises at least one of cyclopropanecarboxylic acid, cyclobutanecarboxylic acid, cyclopentanecarboxylic acid, or cyclopropanedicarboxylic acid.
5. The self-catalyzed composite carbon-based thin film solid liquid composite lubrication system of claim 1, wherein the cycloalkanol comprises at least one of cyclopropyl alcohol, cyclobutyl alcohol, cyclopentyl alcohol, or dihydroxycyclopropyl alcohol.
6. The self-catalyzed composite carbon-based film solid-liquid composite lubrication system according to claim 1, wherein the content of metal oxide in the multi-element doped DLC nano-composite film is 0.1-30wt%.
7. The method for preparing the self-catalyzed composite carbon-based film solid-liquid composite lubrication system of claim 1, comprising:
(1) Preparing an oxide composite carbon-based film, and treating the surface of the titanium alloy by adopting a magnetron sputtering technology to obtain the titanium alloy;
(2) The preparation of the solid-liquid composite lubrication system of the oxide composite carbon-based film is realized by compounding the oxide composite carbon-based film and the composite lubrication liquid by adopting a dipping-lifting method.
8. The method according to claim 7, wherein the thickness of the oxide composite carbon-based thin film is 0.5 to 4 μm.
9. Use of the self-catalyzed composite carbon-based thin film solid-liquid composite lubrication system of claim 1 for enhancing the friction lubrication performance of parts for engines.
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| US20020022129A1 (en) * | 2000-05-09 | 2002-02-21 | Masaki Moronuki | Amorphous hard carbon film, mechanical parts and method for producing amorphous hard carbon film |
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| CN101943214A (en) * | 2003-08-21 | 2011-01-12 | 日产自动车株式会社 | Low-friction sliding mechanism and method for reducing friction between first sliding member and second sliding member |
| CN102337497A (en) * | 2010-07-22 | 2012-02-01 | 中国科学院兰州化学物理研究所 | Method for preparing multi-element doped carbon-based nano composite film integrating functions of antiwear and lubrication |
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| US20020022129A1 (en) * | 2000-05-09 | 2002-02-21 | Masaki Moronuki | Amorphous hard carbon film, mechanical parts and method for producing amorphous hard carbon film |
| JP2005090738A (en) * | 2003-08-13 | 2005-04-07 | Nissan Motor Co Ltd | Rolling bearing |
| CN101943214A (en) * | 2003-08-21 | 2011-01-12 | 日产自动车株式会社 | Low-friction sliding mechanism and method for reducing friction between first sliding member and second sliding member |
| CN101463466A (en) * | 2007-12-18 | 2009-06-24 | 中国科学院兰州化学物理研究所 | Preparation of metal doped diamond-like surface ion liquid lubricant self-assembled lubricating film |
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