CN115260801A - Graphite-based high-temperature lubricating coating, preparation method thereof and lubricating coating - Google Patents
Graphite-based high-temperature lubricating coating, preparation method thereof and lubricating coating Download PDFInfo
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- CN115260801A CN115260801A CN202210909088.3A CN202210909088A CN115260801A CN 115260801 A CN115260801 A CN 115260801A CN 202210909088 A CN202210909088 A CN 202210909088A CN 115260801 A CN115260801 A CN 115260801A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 111
- 239000010439 graphite Substances 0.000 title claims abstract description 111
- 238000000576 coating method Methods 0.000 title claims abstract description 106
- 239000011248 coating agent Substances 0.000 title claims abstract description 101
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- NXMRPJWKUHQMML-UHFFFAOYSA-K [Cr+3].P(=O)([O-])([O-])[O-].[Mg+2] Chemical compound [Cr+3].P(=O)([O-])([O-])[O-].[Mg+2] NXMRPJWKUHQMML-UHFFFAOYSA-K 0.000 claims abstract description 46
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical group O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000853 adhesive Substances 0.000 claims abstract description 33
- 230000001070 adhesive effect Effects 0.000 claims abstract description 33
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 32
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 32
- -1 rare earth fluoride Chemical class 0.000 claims abstract description 32
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 19
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 14
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical group F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 claims abstract description 13
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 27
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 239000000395 magnesium oxide Substances 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 229940117975 chromium trioxide Drugs 0.000 claims description 12
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 12
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims description 12
- 238000001238 wet grinding Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 239000000314 lubricant Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 description 24
- 239000000203 mixture Substances 0.000 description 15
- 239000000243 solution Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 229910019142 PO4 Inorganic materials 0.000 description 9
- 239000008213 purified water Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 3
- 239000012763 reinforcing filler Substances 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a graphite-based high-temperature lubricating coating, a preparation method thereof and a lubricating coating, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 5.0 to 10.0 percent of water-soluble chromium magnesium phosphate, 6.0 to 12.0 percent of graphite, 1 to 6.0 percent of metal oxide, 0.5 to 3.0 percent of nano rare earth fluoride and the balance of water. Wherein the metal oxide is antimony trioxide and/or lead oxide; the nano rare earth fluoride is lanthanum trifluoride and/or cerium trifluoride. The graphite-based high-temperature lubricating coating provided by the invention can be normally used at 510 +/-10 ℃ when applied to an engine, and the adhesive force and the friction resistance meet the requirements.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a graphite-based high-temperature lubricating coating, a preparation method thereof and a lubricating coating.
Background
In order to improve the maneuverability of the engine and reduce the fuel consumption, the requirement of the combustion temperature is higher and higher, however, the too high temperature brings more severe use environment to the metal parts. Parts such as a central pull rod, a power turbine shaft and a low-pressure shaft are heavy parts of an engine, and the parts work in a high-temperature environment for a long time, and the working temperature of the parts is about 510 ℃. Parts such as the central pull rod, the power turbine shaft, the low-pressure shaft and the like are connected by adopting structures such as threads, splines and the like, and the matching surfaces of the threads and the splines often have serious abrasion and sintering adhesion problems during installation, work and disassembly, so that the work efficiency and the service life of key parts are directly influenced. The lubricating technology is generally adopted to solve the problems of the matching surface abrasion and sintering adhesion of the connecting part of the threads and the splines. In a low-temperature environment, a liquid lubrication technology is generally adopted; in high temperature environment, solid lubricant coating technology is usually adopted. When the use temperature exceeds 400 ℃ or more, a solid lubricating and releasing coating technology of an inorganic resin bonding type is generally adopted. The existing solid lubricating anti-sticking coating in China cannot completely meet the use requirements of parts such as a central pull rod and the like in terms of performance.
The lubricating anti-sticking paint is a special paint, and is characterized by that it utilizes adhesive to adhere powdered solid lubricant (such as molybdenum disulfide, graphite and polytetrafluoroethylene) and other reinforced or heat-resisting filler on the metal base material to form a layer of coating so as to reduce friction and raise anti-sticking effect. At present, most of high-temperature lubricating anti-sticking coating adhesives used in the environment with the temperature of more than 400 ℃ adopt inorganic adhesives, and silicate and phosphate are taken as main materials. However, the heat-resistant paint using silicate as an adhesive has poor adhesion, impact resistance and water and oil resistance, and the long-term use temperature is not higher than 500 ℃, so that the use requirement of parts cannot be met. And phosphate is a high-temperature lubricating anti-sticking coating adhesive material.
Disclosure of Invention
The invention provides a graphite-based high-temperature lubricating coating, a preparation method thereof and a lubricating coating, and aims to solve the problem that the adhesion and the friction resistance of a solid lubricating anti-sticking coating on an engine part cannot meet the requirements when the part of an engine in the prior art works at a high temperature of 510 +/-10 ℃.
According to one aspect of the invention, the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 5.0-10.0% of water-soluble chromium magnesium phosphate, 6.0-12.0% of graphite, 1-6.0% of metal oxide, 0.5-3.0% of nano rare earth fluoride and the balance of water, wherein the metal oxide is antimony trioxide and/or lead oxide; the nano rare earth fluoride is lanthanum trifluoride and/or cerium trifluoride.
Further, the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 6-8% of water-soluble chromium magnesium phosphate, 8-10% of graphite, 3-5% of metal oxide, 1-2% of nano rare earth fluoride and the balance of water.
Furthermore, the purity of the graphite is more than 98 percent, and the particle size is less than or equal to 5 mu m; and/or the purity of the metal oxide is more than 99 percent, and the particle size is less than or equal to 5 mu m; and/or the particle size of the nano rare earth fluoride is less than or equal to 60nm.
According to another aspect of the present invention, there is provided a method for preparing the graphite-based high-temperature lubricating coating, comprising the steps of:
(1) Adding phosphoric acid into phosphorus pentoxide, and stirring and mixing in an oil bath to obtain a reactant, wherein the molar ratio of the phosphorus pentoxide to the phosphoric acid is 1 (2.85-3.00);
(2) Under the condition of stirring, dropwise adding a magnesium oxide solution and a chromium trioxide solution into the reactant in sequence, and continuously stirring to obtain chromium magnesium phosphate, wherein PO in the chromium magnesium phosphate4 -3And Cr+6And Mg+2The mol ratio is 1.0 (0.29-0.3) to 0.85-0.9;
(3) Adjusting the solid content of the chromium phosphate magnesium to 39.5-40.5% by using water to obtain a water-soluble chromium phosphate magnesium adhesive;
(4) Mixing graphite, metal oxide and nano rare earth fluoride, and then carrying out wet grinding to obtain a wet grinding material;
(5) And adding the water-soluble chromium phosphate magnesium adhesive and water into the wet grinding material, stirring and filtering to obtain filtrate, namely the graphite-based high-temperature lubricating coating.
Further, the temperature of the oil bath in the step (1) is 140-160 ℃; and/or the stirring time is 100-140 min.
Further, the mass percentage concentration of the magnesium oxide solution in the step (2) is 20-25%; and/or the mass percentage concentration of the chromium trioxide solution is 30-35%.
Further, in the step (2), the stirring is continued for 6 hours or more.
Further, the wet grinding of the graphite, the metal oxide and the nano rare earth fluoride after mixing in the step (4) comprises: mixing graphite, metal oxide and nano rare earth fluoride, adding water and grinding until the particle size is 2-10 mu m.
According to another aspect of the invention, a graphite-based high-temperature lubricating coating is provided, and is formed by spraying the graphite-based high-temperature lubricating coating or the graphite-based high-temperature lubricating coating prepared by the preparation method on the surface of a part.
Further, the spray coating process includes:
(1) Pretreating the surface of the part;
(2) Spraying a graphite-based high-temperature lubricating coating on the surface of the pretreated part;
(3) And (3) placing the sprayed part in the air for more than 5 hours, and then heating and curing to obtain the graphite-based high-temperature lubricating coating.
The invention has the following beneficial effects:
the invention adopts water-soluble chromium magnesium phosphate as an adhesive, on one hand, the chromium magnesium phosphate is considered to have good bonding with metal at high temperature, and on the other hand, the water-soluble chromium magnesium phosphate is also considered to have good film forming property. The metal oxide adopted by the invention is antimony trioxide and/or lead oxide, and the antimony trioxide and/or lead oxide is added, on one hand, the antimony trioxide and the lead oxide can improve the mechanical property (strength) of the lubricating coating so as to improve the bearing capacity of the lubricating coating, on the other hand, the antimony trioxide and the lead oxide and the like have excellent high-temperature oxidation resistance, and when the antimony trioxide, the lead oxide and the like are enriched around graphite in the lubricating coating, the oxidation of the graphite in a high-temperature environment can be effectively prevented, so that the high-temperature mechanical property and the lubricating property of the coating are improved.
According to the invention, the adopted nano rare earth fluoride is lanthanum trifluoride and/or cerium trifluoride, and the addition of the lanthanum trifluoride and/or cerium trifluoride can improve the density and strength of the lubricating coating, so that the wear resistance of the lubricating coating is improved, and on the other hand, in the friction process, the nano particles are adsorbed on the crystal boundary and crystal face of graphite, so that the oxidation of the graphite in a high-temperature environment can be effectively prevented, and the wear resistance and the bearing capacity of the graphite coating are improved.
The graphite-based high-temperature lubricating coating provided by the invention has the following excellent properties:
(1) the heat resistance of the coating of the invention is as follows: the temperature is kept at 510 +/-10 ℃ for 50 hours, the coating is complete, no cracks, no softening, no shedding, no bubbles and the like are generated, and the adhesive force of the coating is less than or equal to 2 grade;
(2) the thermal cycle performance of the coating of the invention is as follows: keeping the temperature at 510 +/-10 ℃ for 10min, taking out, cooling to room temperature for 1 cycle, and performing cycle test for 30 times;
(3) the friction coefficient of the coating is less than or equal to 0.30 at 510 +/-10 ℃, and the wear life of the coating is more than or equal to 1h.
In conclusion, the graphite-based high-temperature lubricating coating provided by the invention can be normally used at 510 +/-10 ℃ when applied to an engine, and the adhesive force and the friction resistance meet the requirements.
Detailed Description
In order to make the objects, technical solutions and advantageous technical effects of the present invention more clear, the present invention is further described in detail with reference to the following embodiments. It should be understood that the embodiments described in this specification are only for the purpose of explaining the present invention and are not intended to limit the present invention.
For the sake of brevity, only some numerical ranges are explicitly disclosed herein. However, any lower limit may be combined with any upper limit to form ranges not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and similarly any upper limit may be combined with any other upper limit to form a range not explicitly recited. Also, although not explicitly recited, each point or individual numerical value between the endpoints of a range is encompassed within that range. Thus, each point or individual value can form a range not explicitly recited as its own lower or upper limit in combination with any other point or individual value or in combination with other lower or upper limits.
In the description herein, it is to be noted that, unless otherwise specified, "above" and "below" are inclusive, and "a plurality" of "one or more" means two or more.
The embodiment of the first aspect of the invention provides a graphite-based high-temperature lubricating coating, which comprises the following raw material components in percentage by mass: 5.0-10.0% of water-soluble chromium magnesium phosphate, 6.0-12.0% of graphite, 1-6.0% of metal oxide, 0.5-3.0% of nano rare earth fluoride and the balance of water, wherein the metal oxide is antimony trioxide and/or lead oxide; the nano rare earth fluoride is lanthanum trifluoride and/or cerium trifluoride.
The phosphate has good bonding with metal at high temperature, the curing temperature in the atmosphere is low, and the coating on the metal substrate does not fall off after repeated thermal shock in a high-temperature environment of 100-800 ℃, so that the phosphate is a better inorganic adhesive, and particularly the chromium phosphate magnesium adhesive with good film forming property and bonding property is an ideal candidate material for serving as a high-temperature lubricating anti-sticking coating adhesive. The invention uses water-soluble chromium magnesium phosphate as adhesive, graphite as graphite-based high-temperature lubricant, metal oxide and nano rare earth fluoride as reinforcing filler, and purified water as diluent to form the graphite-based high-temperature lubricating coating.
The water-soluble chromium magnesium phosphate is used as the adhesive, on one hand, the chromium magnesium phosphate is well bonded with metal at high temperature, on the other hand, the water-soluble chromium magnesium phosphate has good film forming property, and the graphite-based high-temperature lubricating coating can play a good protection role when being applied to engine parts.
The water-soluble chromium magnesium phosphate is 5.0 to 10.0% by mass, for example, 5.0%, 6.0%, 7.0%, 8.0%, 9.0% or 10.0%. The water-soluble chromium magnesium phosphate is used as the adhesive, and the mass percentage of the water-soluble chromium magnesium phosphate can be in any combination range of the above values.
The solid lubricant is a main lubricating substance of a lubricating coating, the graphite serving as the lubricant has excellent lubricating performance at room temperature to 510 ℃, and the graphite has serious oxidation weight loss under the oxidizing environment higher than 510 ℃, so that the mechanical property and the lubricating performance of the graphite are influenced. The metal oxide adopted by the invention is antimony trioxide and/or lead oxide, on one hand, the antimony trioxide and the lead oxide can improve the mechanical property (strength) of the lubricating coating, thereby improving the bearing capacity of the lubricating coating, on the other hand, the antimony trioxide, the lead oxide and the like have excellent high-temperature oxidation resistance, and when the antimony trioxide, the lead oxide and other particles are enriched around graphite in the lubricating coating, the oxidation of the graphite in a high-temperature environment can be effectively prevented, thereby improving the high-temperature mechanical property and the lubricating property of the coating.
The nano rare earth fluoride adopted by the invention is lanthanum trifluoride and/or cerium trifluoride, so that on one hand, the density and the strength of the lubricating coating can be improved, and the wear resistance of the lubricating coating is improved, and on the other hand, in the friction process, the nano particles are adsorbed on the crystal boundary and the crystal face of graphite, so that the oxidation of the graphite in a high-temperature environment can be effectively prevented, and the wear resistance and the bearing capacity of the graphite coating are improved.
The solid lubricant is graphite with the mass percentage of 6.0-12.0%, for example, the mass percentage of the graphite is 6.0%, 7.0%, 8.0%, 9.0%, 10.0%, 11.0% or 12.0%, and the mass percentage of the graphite can be in any combination range of the above values.
The invention adopts 1-6.0% of metal oxide as reinforcing filler, for example, the mass percentage of the metal oxide is 1.0%, 2.0%, 3.0%, 4.0%, 5.0% or 6.0%, and the mass percentage of the metal oxide can be any combination range of the above values.
The invention adopts the nano rare earth fluoride with the mass percentage of 0.5-3.0% as the reinforcing filler, for example, the mass percentage of the nano rare earth fluoride is 0.5%, 0.6%, 0.8%, 1.0%, 2.0% or 3.0%, and the mass percentage of the nano rare earth fluoride can be in any combination range of the above values.
The graphite-based high-temperature lubricating coating provided by the invention also comprises 69-87.5% of water.
In the embodiment of the invention, in order to further improve the comprehensive performance of the graphite-based high-temperature lubricating coating at the high temperature of 510 ℃ and above, the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 6 to 8 percent of water-soluble chromium magnesium phosphate, 8 to 10 percent of graphite, 3 to 5.0 percent of metal oxide, 1 to 2.0 percent of nano rare earth fluoride and the balance of water.
In the embodiment of the invention, the purity of the graphite is more than 98 percent, and the particle size is less than or equal to 5 mu m; and/or the purity of the metal oxide is more than 99 percent, and the particle size is less than or equal to 5 mu m; and/or the particle size of the nano rare earth fluoride is less than or equal to 60nm.
An embodiment of a second aspect of the present invention provides a preparation method of the graphite-based high-temperature lubricating coating, including the following steps:
(1) Adding phosphoric acid into phosphorus pentoxide, and stirring and mixing in an oil bath to obtain a reactant, wherein the molar ratio of the phosphorus pentoxide to the phosphoric acid is 1 (2.85-3.00);
(2) Under the condition of stirring, dropwise adding a magnesium oxide solution and a chromium trioxide solution into the reactant in sequence, and continuously stirring to obtain chromium magnesium phosphate, wherein PO in the chromium magnesium phosphate4 -3And Cr+6And Mg+2The mol ratio is 1.0 (0.29-0.3) to 0.85-0.9;
(3) Adjusting the solid content of the chromium phosphate magnesium to 39.5-40.5% by using water to obtain a water-soluble chromium phosphate magnesium adhesive;
(4) Mixing graphite, metal oxide and nano rare earth fluoride, and then carrying out wet grinding to obtain a wet grinding material;
(5) And adding the water-soluble chromium magnesium phosphate adhesive and water into the wet grinding material, stirring and filtering to obtain filtrate, namely the graphite-based high-temperature lubricating coating.
In the embodiment of the invention, the temperature of the oil bath in the step (1) is 140-160 ℃; and/or the stirring time is 100-140 min.
In the embodiment of the invention, the mass percentage concentration of the magnesium oxide solution in the step (2) is 20-25%; and/or the mass percentage concentration of the chromium trioxide solution is 30-35%.
In the present example, the stirring duration in step (2) was 6 hours or more.
In the embodiment of the invention, the wet grinding after mixing graphite, metal oxide and nano rare earth fluoride in the step (4) comprises the following steps: mixing graphite, metal oxide and nano rare earth fluoride, adding water and grinding until the particle size is 2-10 mu m.
In some embodiments, a graphite-based high-temperature lubricating coating and coating of the present invention is prepared as follows:
(1) Preparing a water-soluble chromium phosphate magnesium adhesive:
weighing phosphorus pentoxide (P) according to a certain proportion2O5)(P2O5And H3PO41, 2.85) into a three-necked flask, and then adding phosphoric acid (H)3PO4) Slowly adding the mixture into the reactor, continuously stirring the mixture in an oil bath at 150 ℃ for 120 minutes, taking the mixture out after the stirring is finished, and standing the mixture to room temperature for later use. Respectively preparing 23.9 percent of magnesium oxide (MgO) aqueous solution and 33.3 percent of chromium trioxide (CrO) by weight percentage3) An aqueous solution. Slowly dripping magnesium oxide solution into a three-neck flask by using a dropper, continuously stirring, adding chromium trioxide solution into the flask after the dripping of the magnesium oxide solution is finished, stirring for more than 6 hours until the mixture is fully reacted, and obtaining PO in the composition of the chromium magnesium phosphate4 -3And Cr+6And Mg+2The molar ratio should be 1.0.29. According to the measurement result, the solid content was adjusted to 40.0% with deionized water and was used.
(2) Preparation of graphite-based high-temperature lubricating coating
Mixing the solid lubricant and other modified fillers according to the proportion of the invention, putting the mixture into a ceramic ball milling tank, adding a proper amount of water for grinding, adding the water-soluble chromium phosphate magnesium adhesive after grinding and dispersing the mixture to the required granularity, adding the rest of water, stirring the mixture uniformly, and filtering the mixture to obtain filtrate, namely the graphite-based high-temperature lubricating coating.
The embodiment of the third aspect of the invention provides a graphite-based high-temperature lubricating coating, which is formed by spraying the graphite-based high-temperature lubricating coating or the graphite-based high-temperature lubricating coating prepared by the preparation method on the surface of a part.
In some embodiments, the spray coating process comprises:
(1) Pretreating the surface of the part;
(2) Spraying a graphite-based high-temperature lubricating coating on the surface of the pretreated part;
(3) And (3) placing the sprayed part in the air for more than 5 hours, and then heating and curing to obtain the graphite-based high-temperature lubricating coating.
In the embodiment of the invention, in order to ensure the uniformity of spraying, the solid content of the graphite-based high-temperature lubricating coating is controlled to be about 20%.
The graphite-based high-temperature lubricating coating provided by the invention can be normally used at 510 +/-10 ℃ when applied to an engine, and the adhesive force and the friction property meet the requirements.
Examples
The present disclosure is more particularly described in the following examples that are intended as illustrations only, since various modifications and changes within the scope of the present disclosure will be apparent to those skilled in the art. Unless otherwise indicated, all parts, percentages, and ratios reported in the following examples are on a weight basis, and all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further treatment, and the equipment used in the examples is commercially available.
Example 1
Preparing a water-soluble chromium phosphate magnesium adhesive: weighing phosphorus pentoxide (P) according to a certain proportion2O5)(P2O5And H3PO41: 2.85), 49.8g, was charged into a three-necked flask, and then 98.0g of phosphoric acid (H) was added thereto3PO4) Slowly adding the mixture into the mixture to obtain a mixture,stirring in 150 deg.C oil bath for 120 min, taking out, and standing to room temperature. Respectively preparing 142.0g of magnesium oxide (MgO) aqueous solution with the weight percentage concentration of 23.9 percent and 33.3 percent of chromium trioxide (CrO)3) 87.1g of aqueous solution. Slowly dripping magnesium oxide solution into a three-neck flask by using a dropper, continuously stirring, adding chromium trioxide solution into the flask after the dripping of the magnesium oxide solution is finished, stirring for more than 6 hours until the mixture is fully reacted, and obtaining PO4 in the composition of the chromium magnesium phosphate-3And Cr+6And Mg+2The molar ratio should be 1.0.29. According to the results of the measurement, the solid content was adjusted to 40.0% with deionized water to 527g in total for use.
Weighing 80.0g of graphite, 40.0g of antimony trioxide and 8.0g of nano lanthanum trifluoride, pouring into a ceramic ball milling tank, adding about 100 g of pure inlet water for grinding, grinding and dispersing to the required granularity, weighing 141g of the chromium magnesium phosphate adhesive, adding the rest of water, stirring uniformly, and filtering to obtain filtrate, namely the graphite-based high-temperature lubricating coating.
Preparing a graphite-based high-temperature lubricating coating on the surface of an engine part:
the graphite-based high-temperature lubricating coating obtained in example 1 was subjected to performance tests, and the test results and test standards are shown in table 1 below.
Table 1 test criteria and test results for example 1
Example 2
The preparation method is the same as that of example 1, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 7.5% of graphite, 5.0% of lead oxide, 1.0% of nano lanthanum trifluoride, 0.5% of nano cerium trifluoride, 6.0% of a chromium phosphate magnesium adhesive and the balance of purified water.
The graphite-based high-temperature lubricating coating obtained in example 2 was subjected to performance tests, and the test results and test standards are shown in table 2 below.
Table 2 test criteria and test results for example 2
Example 3
The preparation method is the same as that of example 1, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 7.5% of graphite, 5.0% of lead oxide, 1.5% of nano cerium trifluoride, 6.0% of chromium magnesium phosphate adhesive and the balance of purified water.
Example 4
The preparation method is the same as that of example 1, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 7.5% of graphite, 5.0% of lead oxide, 1.5% of nano lanthanum trifluoride, 6.0% of chromium phosphate magnesium adhesive and the balance of purified water.
Example 5
The preparation method is the same as that of example 1, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 7.5% of graphite, 3.0% of antimony trioxide, 2.0% of lead oxide, 1.5% of nano cerium trifluoride, 6.0% of chromium phosphate magnesium adhesive and the balance of purified water.
Example 6
The preparation method is the same as that of example 1, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 7.0 percent of graphite, 3.0 percent of antimony trioxide, 2.5.0 percent of lead oxide, 1.5 percent of nano lanthanum trifluoride, 6.0 percent of chromium phosphate magnesium adhesive and the balance of purified water.
Example 7
The preparation method is the same as that of example 1, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 7.5% of graphite, 5.0% of antimony trioxide, 1.5% of nano lanthanum trifluoride, 6.5% of chromium phosphate magnesium adhesive and the balance of purified water.
Example 8
The preparation method is the same as that of example 1, wherein the graphite-based high-temperature lubricating coating comprises the following raw material components in percentage by mass: 7.5% of graphite, 3.0% of antimony trioxide, 2.0% of lead oxide, 0.5% of nano lanthanum trifluoride, 1.0% of nano cerium trifluoride, 6.0% of a chromium magnesium phosphate adhesive and the balance of purified water.
The graphite-based high-temperature lubricating coatings obtained in examples 3 to 8 were subjected to performance tests, and the test results and test standards were as follows in table 3.
TABLE 3 test standards and test results for examples 3-8
Comparative example 1
This comparative example is different from example 1 in that it lacks metal oxide and nano rare earth fluoride, and is the same as example 1.
The coatings obtained in comparative example 1 were subjected to performance tests, the test results and the test criteria are given in table 4 below.
Table 4 test standards and test results for comparative example 1
Comparative example 2
This comparative example is different from example 1 in that nano rare earth fluoride is absent, and the rest is the same as example 1.
The coatings obtained in comparative example 2 were subjected to performance tests, the results and test criteria being given in table 5 below.
TABLE 5 test standards and test results for comparative example 2
Comparative example 3
This comparative example is the same as example 1 except that the metal oxide was absent from the comparative example 1.
The coatings obtained in comparative example 3 were subjected to performance tests, and the test results and test criteria are shown in table 6 below.
TABLE 6 test standards and test results for comparative example 3
Therefore, each component in the invention plays a certain role. Graphite has excellent lubricating properties at room temperature to 510 ℃. The metal oxide improves the lubricity of the coating. The nano rare earth fluorination can improve the wear resistance of the lubricating coating.
While the invention has been described with reference to a preferred embodiment, various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention, and particularly, features shown in the various embodiments may be combined in any suitable manner without departing from the scope of the invention. It is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. The graphite-based high-temperature lubricating coating is characterized by comprising the following raw material components in percentage by mass: 5.0-10.0% of water-soluble chromium magnesium phosphate, 6.0-12.0% of graphite, 1-6.0% of metal oxide, 0.5-3.0% of nano rare earth fluoride and the balance of water, wherein the metal oxide is antimony trioxide and/or lead oxide; the nano rare earth fluoride is lanthanum trifluoride and/or cerium trifluoride.
2. The graphite-based high-temperature lubricating coating as claimed in claim 1, characterized by comprising the following raw material components in percentage by mass: 6-8% of water-soluble chromium magnesium phosphate, 8-10% of graphite, 3-5% of metal oxide, 1-2% of nano rare earth fluoride and the balance of water.
3. The graphite-based high-temperature lubricating coating as claimed in claim 1, wherein the graphite has a purity of > 98% and a particle size of 5 μm or less; the purity of the metal oxide is more than 99 percent, and the particle size is less than or equal to 5 mu m; the particle size of the nano rare earth fluoride is less than or equal to 60nm.
4. A method for preparing a graphite-based high-temperature lubricating coating as claimed in any one of claims 1 to 3, characterized by comprising the steps of:
(1) Adding phosphoric acid into phosphorus pentoxide, and stirring and mixing in an oil bath to obtain a reactant, wherein the molar ratio of the phosphorus pentoxide to the phosphoric acid is 1 (2.85-3.00);
(2) Under the condition of stirring, dropwise adding a magnesium oxide solution and a chromium trioxide solution into the reactant in sequence, and continuously stirring to obtain chromium magnesium phosphate, wherein PO in the chromium magnesium phosphate4 -3、Cr+6And Mg+2The mol ratio is 1 (0.29-0.3) to 0.85-0.9;
(3) Adjusting the solid content of the chromium phosphate magnesium to 39.5-40.5% by using water to obtain a water-soluble chromium phosphate magnesium adhesive;
(4) Mixing graphite, metal oxide and nano rare earth fluoride, and then carrying out wet grinding to obtain a wet grinding material;
(5) And adding the water-soluble chromium phosphate magnesium adhesive and water into the wet grinding material, stirring and filtering to obtain filtrate, namely the graphite-based high-temperature lubricating coating.
5. The method for preparing the graphite-based high-temperature lubricating coating according to claim 4, wherein the temperature of the oil bath in the step (1) is 140-160 ℃; and/or
The stirring time is 100-140 min.
6. The preparation method of the graphite-based high-temperature lubricating coating according to claim 4, wherein the mass percentage concentration of the magnesium oxide solution in the step (2) is 20-25%; and/or
The mass percentage concentration of the chromium trioxide solution is 30-35%.
7. The method for preparing a graphite-based high-temperature lubricating coating according to claim 4, wherein in the step (2), the stirring is continued for 6 hours or more.
8. The method for preparing the graphite-based high-temperature lubricating coating according to the claim 4, wherein the wet grinding after mixing the graphite, the metal oxide and the nano rare earth fluoride in the step (4) comprises the following steps:
mixing graphite, metal oxide and nano rare earth fluoride, adding water and grinding until the particle size is 2-10 mu m.
9. A graphite-based high-temperature lubricating coating, which is characterized in that the graphite-based high-temperature lubricating coating is formed by spraying the graphite-based high-temperature lubricating coating as claimed in any one of claims 1 to 3 or the graphite-based high-temperature lubricating coating prepared by the preparation method as claimed in any one of claims 4 to 8 on the surface of a part.
10. The graphite-based high temperature lubricant coating of claim 9, wherein the spray coating process comprises:
(1) Pretreating the surface of the part;
(2) Spraying a graphite-based high-temperature lubricating coating on the surface of the pretreated part;
(3) And (3) placing the sprayed part in the air for more than 5 hours, and then heating and curing to obtain the graphite-based high-temperature lubricating coating.
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