CN114539922B - Anti-scouring radiation heat-resistant coating for titanium alloy, and preparation method and application thereof - Google Patents

Anti-scouring radiation heat-resistant coating for titanium alloy, and preparation method and application thereof Download PDF

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CN114539922B
CN114539922B CN202011347680.6A CN202011347680A CN114539922B CN 114539922 B CN114539922 B CN 114539922B CN 202011347680 A CN202011347680 A CN 202011347680A CN 114539922 B CN114539922 B CN 114539922B
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coating
titanium alloy
scour
parts
radiation heat
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CN114539922A (en
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王贤明
王飞
吴连锋
宁亮
张燕
易敏华
刘雷雷
卢敏
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Marine Chemical Research Institute Co Ltd
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    • 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
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    • C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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    • B05D2202/00—Metallic substrate
    • B05D2202/30—Metallic substrate based on refractory metals (Ti, V, Cr, Zr, Nb, Mo, Hf, Ta, W)
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    • Y02T50/60—Efficient propulsion technologies, e.g. for aircraft

Abstract

The invention relates to a titanium alloy anti-scouring radiation heat-resistant coating, a preparation method and application thereof, belonging to the field of heat-resistant coatings. The anti-scouring radiation heat-insulating coating for the titanium alloy comprises an adhesive layer primer layer and a high emissivity layer; the bonding layer primer layer is formed by curing bonding layer primer; the high-emissivity layer is formed by curing high-emissivity paint; the thickness of the primer layer of the bonding layer is 2-30 mu m; the thickness of the coating of the high emissivity layer is 20-50 mu m; the infrared emissivity of the anti-scouring radiation heat-insulating coating is more than or equal to 85%, the adhesive force of the coating on the titanium alloy is more than or equal to 4.0MPa, and the adhesive force of the coating after 700 ℃/10min heat treatment is more than or equal to 2.0MPa; the coating can be well attached to titanium alloy, can still have better attachment and good high-speed airflow scouring resistance after being heated at high temperature, is convenient to construct by adopting air spraying, and is worthy of popularization and application.

Description

Anti-scouring radiation heat-resistant coating for titanium alloy, and preparation method and application thereof
Technical Field
The invention relates to the field of heat-resistant coatings, in particular to a titanium alloy anti-scouring radiation heat-resistant coating and a preparation method and application thereof.
Background
Titanium alloy has advantages of heat resistance, high specific strength, corrosion resistance and the like, and is widely applied to the aviation field, such as parts and machine bodies of aeroengines requiring heat resistance and high strength. During high-speed flight, the surface of the machine body is heated due to pneumatic friction, so that the surface temperature of the machine body rises to hundreds of degrees. At the same time, long-time solar radiation can heat the surface of the machine body. Both sources of heat can cause high temperatures on the surfaces of the electronic components during performance of the task, which can affect the proper operation of the internal electronic components. Most importantly, the heat-resistant temperature of the titanium alloy is limited, the titanium alloy is subjected to oxygen embrittlement at the high temperature of more than 600 ℃, the mechanical property of the titanium alloy is reduced, the safety is seriously influenced, and the protection by adopting the heat-resistant coating is one of the most effective ways for solving the problem.
The high infrared emissivity coating is a radiation heat-resistant coating material, is widely applied to a heat-resistant system, and can radiate heat generated by pneumatic heating in an infrared radiation mode to reduce the temperature of the surface of an aircraft. The organic high-emissivity coating material using the high-temperature resistant resin as a film forming material has the advantages of simple preparation method, convenient construction and the like, is widely used, the emissivity of the existing organic high-emissivity coating can reach more than 0.8, the temperature resistance is generally more than 500 ℃, and the short-time use temperature can reach 1300 ℃. However, after a short time of high temperature, the adhesion of the coating will be greatly reduced, and the coating may crack, fall off, etc. when the task is performed again, so that the substrate directly faces the aerodynamic high temperature, which will greatly affect the anti-scouring performance, reliability, and safety of the aircraft.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a anti-scouring radiation heat-resistant coating for titanium alloy. In particular to a scour-resistant radiation heat-resistant coating for titanium alloy, a preparation method and application thereof. The technical scheme of the invention adopts a mode of combining the bonding layer primer and the high-emissivity finish paint, has high bonding force with titanium alloy and high-temperature resistance treatment, and solves the problems that the bonding strength of the high-emissivity coating after high temperature is reduced and the high-emissivity coating is easy to fall off in the high-speed flight process.
The invention aims to provide a titanium alloy anti-scouring radiation heat-resistant coating which is good in high-temperature adhesion and resistant to high-speed airflow scouring. The coating comprises a primer layer of an adhesive layer for improving high-temperature adhesion and a high-emissivity layer for playing a role of radiation heat insulation. Wherein the bonding layer primer layer is formed by curing bonding layer primer; the high-emissivity layer is formed by curing high-emissivity paint. The bonding layer primer can be composed of polysilazane, high-temperature resistant filler and the like; the high emissivity coating can be composed of high temperature resistant resin, high emissivity filler, high temperature resistant filler and the like.
In particular, the method comprises the steps of,
the primer layer of the adhesive layer may have a coating thickness of 2 to 30 μm, preferably a thickness of 5 to 20 μm;
the high emissivity layer may have a coating thickness of 20 to 50 μm, preferably a thickness of 20 to 40 μm;
the infrared (8-14 mu m) emissivity of the anti-scouring radiation heat-insulating coating is more than or equal to 85%, so that the radiation heat-insulating purpose can be achieved; the adhesive force (drawing method) of the coating on the titanium alloy is more than or equal to 4.0MPa, and after 700 ℃/10min heat treatment, the adhesive force of the coating can be more than or equal to 2.0MPa, and good adhesion is still maintained.
Preferably, the fineness of the adhesive layer primer is less than 20 μm.
Wherein, the liquid crystal display device comprises a liquid crystal display device,
the bonding layer primer can comprise the following components in parts by weight:
100 parts by weight of polysilazane,
10 to 60 parts by weight, preferably 20 to 50 parts by weight, of a high temperature resistant filler.
In particular, the method comprises the steps of,
the structural unit of the polysilazane may be of the general formula (I),
Figure BDA0002800428410000021
wherein R is 1 is-CH 3 or-CH 2 CH 3 ，R 2 is-CH 3 Or H.
The molecular weight of the polysilazane may be 300 to 15000, preferably 600 to 10000.
The high-temperature-resistant filler in the bonding layer primer can be at least one of nano silicon dioxide powder, silicon carbide, boron nitride, ferric oxide and graphene; preferably, the high temperature resistant filler in the bonding layer primer may comprise a mixture of nano silicon dioxide powder, silicon carbide, iron oxide, graphene, boron nitride; wherein, the weight ratio of the nano silicon dioxide powder, silicon carbide, ferric oxide, boron nitride and graphene is (10-20): (5-15): (1-8): (0-15): (0-5); preferably (10 to 16): (5-10): (2-6): (0-10): (0-4).
In some implementations of the invention, the bond coat primer may further comprise an ultra-fine glass frit;
the amount of the ultra-fine glass powder may be 10 to 50 parts by weight, preferably 10 to 30 parts by weight, based on 100 parts by weight of the polysilazane;
and/or the number of the groups of groups,
the superfine glass powder in the bonding layer primer can be selected from one or more of superfine low-melting-point glass powder with different melting points above 600 ℃;
the mesh number of the selected superfine glass powder can be 1000-10000 meshes, and the preferable mesh number is 1000-5000 meshes.
In some implementations of the invention, the bond coat primer may further comprise a diluent, which may be used in an amount of 0 to 60 parts by weight based on 100 parts by weight of the polysilazane;
the diluent in the bond coat primer may be selected from non-polar solvents; preferably, the nonpolar solvent may be selected from one or two or more of xylene, n-butyl ether, methylene chloride, etc.
The high emissivity coating may comprise an a component and a B component;
the component A can comprise the following components in parts by weight:
100 parts by weight of a high-temperature resistant resin solution, wherein the concentration of the high-temperature resistant resin solution can be 40-60%wt;
30 to 150 parts by weight, preferably 60 to 130 parts by weight,
20 to 100 parts by weight, preferably 30 to 80 parts by weight,
the component B is a curing agent;
the curing agent can be used in an amount of 0.5 to 8 parts by weight, preferably 0.5 to 5 parts by weight, based on 100 parts by weight of the high-temperature resistant resin solution in the component A; the curing agent of the component B can be at least one selected from butyl titanate, stannous octoate, dibutyl tin dilaurate and diethyl tin dioctoate.
Preferably, the method comprises the steps of,
the fineness of the A component of the high emissivity coating can be 40-120 mu m, preferably 60-100 mu m.
In the high emissivity coating of the invention, the high temperature resistant resin solution can be boric acid modified silicone resin solution;
the B/Si molar ratio of the boric acid modified silicone resin can be 1 (2-7), preferably 1 (3-6); and/or the number of the groups of groups,
the phenyl/Si molar ratio of the boric acid modified silicone resin may be 0.15 to 0.6, preferably 0.2 to 0.4; and/or the number of the groups of groups,
the molar ratio R/Si of the boric acid modified silicone resin can be 1.2-1.8, preferably 1.4-1.6;
preferably, the method comprises the steps of,
the structural units of the boric acid modified silicone resin may comprise the following general formula (II):
Figure BDA0002800428410000041
the high-temperature resistant resin in the high-emissivity coating can be prepared by a preparation method comprising the following steps:
1) Blending and hydrolyzing components including methyltriethoxysilane, phenyltriethoxysilane, dimethyldiethoxysilane, diphenyldiethoxysilane, boric acid, deionized water and ethanol to obtain a prepolymer; preferably, the weight ratio of methyltriethoxysilane, phenyltriethoxysilane, dimethyldiethoxysilane, diphenyldiethoxysilane, boric acid, deionized water and ethanol is as follows: (40-70 parts) of: (30-50 parts of: (25-40 parts) of: (20-40 parts) of: (10-20 parts of: (100-120 parts of: (180-220 parts);
2) Vacuum distilling to remove water and ethanol, removing volatile components, and adding a solvent to obtain the high-temperature-resistant resin solution;
preferably, the method comprises the steps of,
in the step 1), the hydrolysis temperature can be 70-90 ℃ and the hydrolysis time is 2-4 h;
in the step 2), the temperature of the reduced pressure distillation may be 70 to 80 ℃; the solvent can be selected from at least one of dimethylbenzene and gasoline; the concentration of the resulting high temperature resistant resin solution may be 40 to 60wt%.
The high emissivity filler in the high emissivity coating may comprise Fe 2 O 3 、MnO 2 、SiB 4 At least one of CuO, graphene; preferably, the high emissivity filler may comprise Fe 2 O 3 、MnO 2 、SiB 4 Mixtures of CuO, graphene; wherein Fe is 2 O 3 ：MnO 2 ：SiB 4 : cuO: the weight ratio of the graphene can be (20-50): (5-20): (40-70): (5-10): (5-10).
The high-temperature-resistant filler in the high-emissivity coating can be one or more than two of nano silicon dioxide, silicon carbide (SiC), boron Nitride (BN), wollastonite and talcum powder; preferably, the high-temperature resistant filler in the high-emissivity coating comprises a mixture of nano silicon dioxide, silicon carbide, boron nitride, wollastonite and talcum powder; wherein, nano silicon dioxide: silicon carbide (SiC): boron Nitride (BN): wollastonite: the weight ratio of talcum powder can be (10-20): (10-20): (5-10): (0-15): (0-15).
In some implementations of the invention, the a component of the high emissivity coating may further comprise a diluent, which may be used in an amount of 20 to 120 parts by weight based on 100 parts by weight of the high temperature resistant resin solution;
the diluent of the high-emissivity coating can be selected from one or two of dimethylbenzene, solvent oil and cyclohexane; preferably, the solvent oil may be at least one selected from the group consisting of solvent gasoline, solvent oil No. 120, and solvent oil No. 180.
In some implementations of the invention, the a component of the high emissivity coating may also include a fluxing agent; the flux may be used in an amount of 1 to 15 parts by weight, preferably 3 to 10 parts by weight, based on 100 parts by weight of the high temperature resistant resin solution; the fluxing agent of the high-emissivity coating can be one or two of glass powder, lead and borax; the fluxing agent is favorable for secondary film formation. Wherein the particle size of the glass frit may be 200 to 1000 mesh, preferably 400 to 800 mesh.
The second object of the invention is to provide a preparation method of the anti-scouring radiation heat-resistant coating for titanium alloy, which comprises the following steps:
firstly, spraying and curing the bonding layer primer to obtain a bonding layer primer layer, and then spraying and curing the high-emissivity coating to obtain a high-emissivity layer, thus obtaining the anti-scouring radiation heat-insulating coating;
preferably, the preparation method may comprise the steps of:
1) The construction of the primer layer of the bonding layer comprises the following steps: firstly, carrying out sand blasting treatment on the titanium alloy to remove an oxide layer, carrying out air spraying on the primer of the bonding layer, adjusting viscosity before spraying, drying the surface of the primer after finishing spraying, and heating and curing to obtain a primer coating;
2) The construction of the high emissivity layer comprises the following steps: and (3) on the basis of the primer coating in the step (1), carrying out air spraying on the high-emissivity coating, uniformly mixing the component A and the component B before spraying, regulating the viscosity, carrying out surface drying on the sprayed coating, and heating and curing to obtain a high-emissivity layer.
Wherein, the liquid crystal display device comprises a liquid crystal display device,
in the construction of the primer layer of the bonding layer in the step 1),
the viscosity can be adjusted to 10-30 s (measured by 4 cups) by adopting a diluent before spraying, and the viscosity can be preferably 12-20 s (measured by 4 cups); and/or the number of the groups of groups,
the air spraying can be performed by adopting a small-caliber spray gun; wherein, the caliber of the small caliber spray gun can be 0.3-1.2 mm, and the caliber is preferably 0.5-0.8 mm; and/or the number of the groups of groups,
the surface drying temperature can be room temperature, and the drying time is 1-4 hours; and/or the number of the groups of groups,
the conditions of the heat curing may include: the temperature is 120-150 ℃ and the time is 30-90 min.
In the construction of the high emissivity layer in the step 2),
the viscosity can be adjusted to 15-40 s (measured by 4 cups) by using a diluent, and preferably the viscosity is 20-30 s (measured by 4 cups);
and/or the number of the groups of groups,
the air spraying is carried out by adopting a spray gun; the caliber of the spray gun is 0.5-0.8 mm;
and/or the number of the groups of groups,
the surface drying temperature is room temperature, and the drying time is 1-4 hours; and/or the number of the groups of groups,
the conditions for heat curing include: the temperature is 180-200 ℃ and the time is 2-4 hours.
Wherein, the liquid crystal display device comprises a liquid crystal display device,
the bonding layer primer is a single component, and the preparation method of the bonding layer primer can comprise the following steps:
the polysilazane-containing high-temperature resistant filler is obtained by blending and dispersing components comprising the polysilazane, the high-temperature resistant filler and the diluent;
the blending may be at a high speed stirring, the stirring speed may be 1000 to 3000rpm, preferably the stirring speed may be 1500 to 2000rpm.
The preparation method of the component A of the high-emissivity coating can comprise the following steps:
the high-temperature resistant resin solution, the high-emissivity filler, the high-temperature resistant filler, the fluxing agent and the diluent are ground and blended to prepare the high-temperature resistant resin composition; preferably, the milling blend uses 2mm zirconium beads and 1mm zirconium beads as milling media, with a milling speed of 1000 to 3000rpm, preferably 1500 to 2200rpm.
The blending equipment or the reaction equipment in the preparation method of the invention is common blending equipment or reaction equipment in the prior art.
The primer is used for improving the adhesive strength of the high-emissivity coating and the titanium alloy, and is mainly characterized in that the adhesive strength of the high-emissivity coating is still higher after the high-temperature coating is used for a system of the invention. The high-temperature-resistant high-emissivity coating prepared by adopting boric acid modified organic silicon resin, an optimized high-emissivity filler system and the like endows the coating with high-emissivity characteristics, and the high-temperature-resistant adhesive layer primer prepared by taking polysilazane as a film forming material and adding the high-temperature-resistant filler and the like improves the high-temperature adhesive strength of the high-emissivity layer and the titanium alloy. The high-temperature-resistant bonding layer primer has strong adhesive force with titanium alloy, good high-temperature resistance and high coating compactness, and can be sintered with the high-temperature-resistant high-emissivity layer for secondary film forming at high temperature, thereby playing a role in connecting the high-emissivity layer with the titanium alloy.
The invention also aims to provide the application of the anti-scouring radiation heat-resistant coating for the titanium alloy or the coating prepared according to the preparation method in high-speed aircrafts and weapons. The coating disclosed by the invention is suitable for conventional titanium alloys in the field, in particular conventional high-temperature-resistant titanium alloys.
The coating provided by the invention can be well attached to titanium alloy, can still have good adhesion and good high-speed airflow scouring resistance after being heated at high temperature, is convenient to construct by adopting air spraying, and is suitable for heat protection of titanium alloy structural members of high-speed aircrafts and the like.
Drawings
FIG. 1 is a schematic view of a titanium alloy anti-scour radiant heat barrier coating according to the present invention; wherein 1 is a high emissivity layer; 2 is an adhesive layer primer layer; 3 is a base material;
FIGS. 2 and 3 are partial magnified photographs of adhesion (pullout) tests before and after the coating of example 1 was subjected to 700℃/10min, respectively;
fig. 4 and 5 are partial enlarged photographs of adhesion (drawing) tests before and after the coating of comparative example 1 was subjected to 700 c/10 min, respectively.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The raw materials used in the examples are all commercially available.
The drawing process used in the examples was carried out according to the test method of the standard GB/T5210-2006 paint and varnish pull-off test.
Example 1
The anti-scour radiation heat-resistant coating comprises an adhesive layer primer layer and a high-emissivity coating layer, and the composition preparation method of the adhesive layer primer layer and the high-emissivity coating layer is as follows: (unless otherwise specified, the parts in the formulation of examples are parts by weight.)
The formula of the primer of the bonding layer is as follows: polysilazane (100 parts; molecular weight: 900, viscosity 50cp, german watt), ultrafine glass powder (1000 mesh, 20 parts), nano silicon dioxide powder (10 parts), ultrafine silicon carbide micropowder (5 parts), ferric oxide (5 parts), graphene (3 parts), xylene (25 parts).
The preparation process of the primer comprises the following steps: the polysilazane, the superfine glass powder, the nano silicon dioxide powder and the superfine silicon carbide micro powder are weighed according to the formula, and are prepared by high-speed stirring and mixing after adding a proper amount of dimethylbenzene, wherein the stirring speed is 2000rpm, the time is 60min, and the fineness is 5 mu m.
The construction process of the primer comprises the following steps: (1) cleaning and degreasing the titanium alloy, and sandblasting; (2) Adding proper amount of dimethylbenzene, and adjusting the viscosity to 12s (coating 4); (3) Spraying the powder onto the surface of the sandblasted titanium alloy with the caliber of 0.5mm, performing surface drying at room temperature for 2 hours, and performing heating solidification at 120 ℃/30min, wherein the dry film thickness is 15 mu m.
The formula of the high emissivity coating comprises the following components: (1) A component: boric acid modified silicone resin solution (100 parts), fe 2 O 3 (30 parts), mnO 2 (6 parts), siB 4 (50 parts), cuO (6 parts), graphene (5 parts), nano silicon dioxide (10 parts), siC (15 parts), BN (5 parts), glass powder (400 meshes, 3 parts) and xylene (80 parts); (2) component B: butyl titanate (5 parts).
The preparation process of the boric acid modified silicone resin solution in the component A of the high-emissivity coating comprises the following steps: 1) Methyl triethoxysilane (599.1 g), phenyl triethoxysilane (346.1 g), dimethyl diethoxysilane (332.1 g), diphenyl diethoxysilane (261.5 g), boric acid powder (123.6 g), deionized water (1 kg) and ethanol (2 kg) are added into a reaction kettle, a proper amount of hydrochloric acid aqueous solution is added dropwise after the temperature is 75 ℃, and the hydrolysis time is 3 hours; 2) After the hydrolysis, water and ethanol were removed by distillation under reduced pressure at 70℃and xylene was added after removal of volatiles to give a 50% strength by weight solution of the high temperature resin.
The preparation process of the component A of the high-emissivity coating comprises the following steps: (1) Weighing boric acid modified silicone resin solution and Fe according to a formula 2 O 3 、MnO 2 、SiB 4 CuO, graphene, nano silicon dioxide, siC, BN, glass frit; (2) After adding a proper amount of dimethylbenzene, adopting grinding and blending, wherein the grinding rotating speed is 1800rpm, the time is 60min, and the fineness of the component A is 60 mu m.
The construction process of the high-emissivity coating comprises the following steps: (1) slightly polishing by using fine sand paper with 1200 meshes; (2) Mixing component A and component B manually, adding appropriate amount of xylene, and adjusting viscosity to 20s (coating 4); (3) Spraying by using a spray gun with the caliber of 0.5mm, drying at room temperature for 2 hours, and heating and curing at the speed of 200 ℃ per 2 hours, wherein the thickness of the coating is 20 mu m.
After the coating is completely cured, an emissivity tester is adopted to test the emissivity of the coating to be 0.91, a drawing method is adopted to test the adhesive force to be 4.7MPa, and after the coating is heated by a muffle furnace at 700 ℃/10min, the test adhesive force (drawing method) is 2.6MPa, so that the anti-scouring performance of the coating and the safety of a high-speed aircraft can be ensured (see fig. 2 and 3).
Example 2
The anti-scour radiation heat-resistant coating comprises an adhesive layer primer layer and a high-emissivity coating layer, and the composition preparation method of the adhesive layer primer layer and the high-emissivity coating layer is as follows:
the formula of the primer of the bonding layer is as follows: polysilazane (molecular weight: 700, viscosity: 15cp,100 parts), ultrafine glass powder (2000 mesh, 10 parts), nanosilica powder (10 parts), ultrafine silicon carbide micropowder (5 parts), ferric oxide (5 parts), xylene (10 parts).
The preparation process of the primer described above was the same as in example 1, with a fineness of 5 μm.
The primer was prepared in the same manner as in example 1, and the dry film thickness was 10. Mu.m.
The formula of the high emissivity coating comprises the following components: (1) A component: boric acid modified silicone resin solution (100 parts), fe 2 O 3 (40 parts), mnO 2 (10 parts), siB 4 (40 parts), cuO (5 parts), graphene (8 parts), nano silicon dioxide (10 parts), siC (15 parts), BN (5 parts), glass powder (5 parts, 600 meshes) and xylene (90 parts); (2) component B: butyl titanate (5 parts).
The preparation process of the boric acid modified silicone resin solution in the component A of the high-emissivity coating comprises the following steps: 1) Methyltriethoxysilane (513.5 g), phenyltriethoxysilane (461.5 g), dimethyldiethoxysilane (284.6 g), diphenyldiethoxysilane (348.7 g), boric acid powder (123.6 g), deionized water (1.1 kg) and ethanol (2.2 kg) are weighed according to a designed proportion, added into a reaction kettle, and added with a proper amount of hydrochloric acid aqueous solution dropwise after the temperature is 85 ℃ for 2 hours; 2) After the hydrolysis was completed, water and ethanol were removed by distillation under reduced pressure at 75℃and xylene was added after the volatiles were removed to obtain a high temperature resistant resin solution having a concentration of 50% by weight.
The preparation process of the component A of the high emissivity coating is the same as that of the example 1, and the fineness of the component A is 80 mu m.
The construction process and parameters of the high emissivity coating were the same as in example 1, the thickness of the coating being 30 μm.
After the above coating was completely cured, the emissivity was 0.90, the coating adhesion (drawing method) was 5.3MPa, and the adhesion after heating was 2.9MPa, as measured in the same manner as in example 1.
Example 3
The anti-scour radiation heat-resistant coating comprises an adhesive layer primer layer and a high-emissivity coating layer, and the composition preparation method of the adhesive layer primer layer and the high-emissivity coating layer is as follows:
the formula of the primer of the bonding layer is as follows: polysilazane (molecular weight: 1200, viscosity: 100cp,100 parts), ultrafine glass powder (2000 mesh, 10 parts), nanosilica powder (15 parts), ultrafine silicon carbide micropowder (8 parts), ferric oxide (5 parts), xylene (30 parts).
The preparation process of the primer described above was the same as in example 1, with a fineness of 8. Mu.m.
The primer was applied in the same manner as in example 1, with a dry film thickness of 15. Mu.m.
The formula of the high emissivity coating comprises the following components: (1) A component: the same as in example 2; (2) component B: butyl titanate (5 parts).
The preparation process of the component A of the high emissivity coating is the same as that of the example 1, and the fineness of the component A is 80 mu m.
The construction process and parameters of the high emissivity coating were the same as in example 1, the thickness of the coating being 30 μm.
After the above coating was completely cured, the emissivity was 0.89, the coating adhesion (drawing method) was 4.1MPa, and the adhesion after heating was 2.2MPa, as measured in the same manner as in example 1.
Example 4
The anti-scour radiation heat-resistant coating comprises an adhesive layer primer layer and a high-emissivity coating layer, and the composition preparation method of the adhesive layer primer layer and the high-emissivity coating layer is as follows:
the formula of the primer of the bonding layer is as follows: polysilazane (molecular weight: 900, viscosity: 50cp,100 parts), ultrafine glass powder (1000 mesh, 20 parts), nanosilica powder (10 parts), ultrafine silicon carbide micropowder (5 parts), ferric oxide (5 parts), BN (5 parts), xylene (40 parts).
The preparation process of the primer described above was the same as in example 1, with a fineness of 5 μm.
The primer was applied in the same manner as in example 1, with a dry film thickness of 12. Mu.m.
The formula of the high emissivity coating comprises the following components: (1) A component: boric acid modified silicone resin solution (100 parts), fe 2 O 3 (40 parts), mnO 2 (10 parts), siB 4 (60 parts), cuO (8 parts), graphene (9 parts), siC (15 parts), nano silicon dioxide powder (10 parts), BN (5 parts), glass powder (8 parts, 400 meshes) and xylene (95 parts); (2) component B: butyl titanate (5 parts).
The preparation process of the boric acid modified silicone resin solution in the component A of the high-emissivity coating comprises the following steps: 1) Methyltriethoxysilane (614.1 g), phenyltriethoxysilane (354.8 g), dimethyldiethoxysilane (340.4 g), diphenyldiethoxysilane (268.0 g), boric acid powder (112.4 g), deionized water (1 kg) and ethanol (2.2 kg) are weighed according to a designed proportion, added into a reaction kettle, and added with a proper amount of hydrochloric acid aqueous solution dropwise after the temperature is 75 ℃ for 4 hours; 2) After the hydrolysis was completed, water and ethanol were removed by distillation under reduced pressure at 80℃and xylene was added after the volatiles were removed to obtain a high temperature resistant resin solution having a concentration of 50% by weight.
The preparation process of the component A of the high emissivity coating is the same as that of the example 1, and the fineness of the component A is 80 mu m.
The construction process and parameters of the high emissivity coating were the same as in example 1, the thickness of the coating being 30 μm.
After the above coating was completely cured, the emissivity was 0.92, the coating adhesion (drawing method) was 4.9MPa, and the adhesion (drawing method) after heating was 2.7MPa, as measured in the same manner as in example 1.
Comparative example 1
To compare the advantages of the high temperature adhesion of the anti-scour radiation thermal barrier coating, the high emissivity coating of example 1 was sprayed onto the grit blasted titanium alloy substrate and tested for adhesion after high temperature heating.
The preparation process and the construction process of the high emissivity coating in comparative example 1 are the same as in example 1, except that in comparative example 1, no primer for the adhesive layer was used. After the above coating was completely cured, the emissivity was measured to be 0.85 by the same method as in example 1, the coating adhesion (drawing method) was 3.6MPa, and the adhesion after heating was 0.7MPa (see fig. 4 and 5).
As can be seen from the comparison of fig. 2 to 5, the coating residue after the drawing test at 700 ℃ is different in example 1 compared with comparative example 1, and the adhesion is poor after heating without primer in comparative example 1; in the embodiment 1 of the application, a part of the coating still remains on the substrate and the obtained drawing strength is higher, so that the requirement of resisting the shearing of the second flight can be met.

Claims (44)

1. A titanium alloy anti-scouring radiation heat-insulating coating is characterized by comprising an adhesive layer primer layer and a high emissivity layer;
the bonding layer primer layer is formed by curing bonding layer primer;
the high-emissivity layer is formed by curing high-emissivity paint;
the thickness of the primer layer of the bonding layer is 2-30 mu m;
the thickness of the coating of the high emissivity layer is 20-50 mu m;
the infrared emissivity of the anti-scouring radiation heat-insulating coating is more than or equal to 85%, the adhesive force of the coating on the titanium alloy is more than or equal to 4.0MPa, and the adhesive force of the coating after 700 ℃/10min heat treatment is more than or equal to 2.0MPa;
the bonding layer primer comprises the following components in parts by weight:
100 parts by weight of polysilazane,
10 to 60 parts by weight of high-temperature resistant filler,
the molecular weight of polysilazane is 300-15000;
the high emissivity coating comprises a component A and a component B;
the component A comprises the following components in parts by weight:
100 parts by weight of a high temperature resistant resin solution,
30 to 150 parts by weight of a filler with high emissivity,
20 to 100 parts by weight of high-temperature resistant filler,
the component B is a curing agent;
in the high-emissivity coating, the high-temperature resistant resin solution is boric acid modified silicone resin solution;
the structural unit of the boric acid modified silicone resin comprises the following general formula (II):
Figure FDA0004233039300000021
2. the anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein: the thickness of the primer layer of the bonding layer is 5-20 mu m;
the coating thickness of the high emissivity layer is 20-40 mu m.
3. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein: the fineness of the bonding layer primer is lower than 20 mu m.
4. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein: the bonding layer primer comprises the following components in parts by weight:
100 parts by weight of polysilazane,
20-50 parts of high-temperature resistant filler.
5. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein: the molecular weight of polysilazane is 600-10000.
6. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein: the high emissivity coating comprises a component A and a component B;
the component A comprises the following components in parts by weight:
100 parts by weight of high-temperature resistant resin solution, wherein the concentration of the high-temperature resistant resin solution is 40-60%wt; 60 to 130 parts by weight of high emissivity filler,
30 to 80 parts by weight of high-temperature resistant filler,
the component B is a curing agent;
the usage amount of the curing agent is 0.5-8 parts by weight based on 100 parts by weight of the high-temperature resistant resin solution in the component A.
7. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 6, wherein:
the usage amount of the curing agent is 0.5-5 parts by weight based on 100 parts by weight of the high-temperature resistant resin solution in the component A.
8. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein:
the fineness of the component A of the high emissivity coating is 40-120 mu m.
9. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 8, wherein:
the fineness of the component A of the high emissivity coating is 60-100 mu m.
10. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein:
the high-temperature-resistant filler in the bonding layer primer is at least one selected from nano silicon dioxide powder, silicon carbide, boron nitride, ferric oxide and graphene.
11. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 10, wherein:
the high-temperature-resistant filler in the bonding layer primer comprises a mixture of nano silicon dioxide powder, silicon carbide, ferric oxide, graphene and boron nitride; wherein, the weight ratio of the nano silicon dioxide powder, silicon carbide, ferric oxide, boron nitride and graphene is (10-20): (5-15): (1-8): (0-15): (0-5).
12. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 11, wherein:
the weight ratio of the nano silicon dioxide powder to the silicon carbide to the iron oxide to the boron nitride to the graphene is (10-16): (5-10): (2-6): (0-10): (0-4).
13. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, characterized in that the bond coat primer contains ultrafine glass powder;
the superfine glass powder is used in an amount of 10-50 parts by weight based on 100 parts by weight of polysilazane.
14. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 13, wherein:
the mesh number of the selected superfine glass powder is 1000-10000 meshes.
15. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 13, wherein:
the superfine glass powder is used in an amount of 10-30 parts by weight based on 100 parts by weight of polysilazane.
16. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 13, wherein:
the mesh number of the selected superfine glass powder is 1000-5000 meshes.
17. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein:
the high-temperature resistant resin in the high-emissivity coating is prepared by a preparation method comprising the following steps:
1) Blending and hydrolyzing components including methyltriethoxysilane, phenyltriethoxysilane, dimethyldiethoxysilane, diphenyldiethoxysilane, boric acid, deionized water and ethanol to obtain a prepolymer;
2) And (3) distilling under reduced pressure, and adding a solvent to obtain the high-temperature resistant resin solution.
18. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 17, wherein:
the weight ratio of the methyltriethoxysilane, the phenyltriethoxysilane, the dimethyldiethoxysilane, the diphenyldiethoxysilane, the boric acid, the deionized water and the ethanol is as follows: (40-70 parts) of: (30-50 parts of: (25-40 parts) of: (20-40 parts) of: (10-20 parts of: (100-120 parts of: (180-220 parts).
19. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 17, wherein:
in the step 1), the hydrolysis temperature is 70-90 ℃ and the hydrolysis time is 2-4 h;
in the step 2), the temperature of the reduced pressure distillation is 70-80 ℃; the solvent is selected from at least one of dimethylbenzene and gasoline; the concentration of the obtained high-temperature resistant resin solution is 40-60 wt%.
20. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein:
the high emissivity filler in the high emissivity coating comprises Fe 2 O 3 、MnO 2 、SiB 4 At least one of CuO and graphene.
21. The anti-scour radiation heat-shielding coating for titanium alloy according to claim 20, wherein:
the high emissivity filler in the high emissivity coating comprises Fe 2 O 3 、MnO 2 、SiB 4 Mixtures of CuO, graphene;
wherein Fe is 2 O 3 ：MnO 2 ：SiB 4 : cuO: the weight ratio of the graphene is (20-50): (5-20): (40～70)：(5～10)：(5～10)。
22. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein:
the high-temperature-resistant filler in the high-emissivity coating is one or more than two selected from nano silicon dioxide, silicon carbide, boron nitride, wollastonite and talcum powder.
23. The anti-scour radiant heat barrier coating for a titanium alloy according to claim 22, wherein:
the high-temperature resistant filler in the high-emissivity coating comprises a mixture of nano silicon dioxide, silicon carbide, boron nitride, wollastonite and talcum powder;
wherein, nano silicon dioxide: silicon carbide (SiC): boron Nitride (BN): wollastonite: the weight of talcum powder is (10-20): (10-20): (5-10): (0-15): (0-15).
24. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein:
the component A in the high emissivity coating comprises a fluxing agent, wherein the amount of the fluxing agent is 1-15 parts by weight based on 100 parts by weight of the high temperature resistant resin solution;
the fluxing agent of the high emissivity coating is one or two selected from glass powder, lead and borax.
25. The anti-scour radiant heat barrier coating for a titanium alloy according to claim 24, wherein:
the amount of the fluxing agent is 3-10 parts by weight based on 100 parts by weight of the high-temperature resistant resin solution.
26. The anti-scour radiant heat barrier coating for a titanium alloy according to claim 24, wherein:
the particle size of the glass powder is 200-1000 meshes.
27. The anti-scour radiant heat barrier coating for a titanium alloy according to claim 26, wherein:
the particle size of the glass powder is 400-800 meshes.
28. The anti-scour radiation heat-insulating coating for titanium alloy according to claim 1, wherein:
the curing agent of the component B is at least one selected from butyl titanate, stannous octoate, dibutyl tin dilaurate and diethyl tin dioctanoate.
29. The method for producing a anti-scour radiation heat-shielding coating for titanium alloy according to any one of claims 1 to 28, characterized by comprising the steps of:
and spraying and curing the bonding layer primer to obtain a bonding layer primer layer, and then spraying and curing the high-emissivity coating to obtain a high-emissivity layer to obtain the anti-scouring radiation heat-insulating coating.
30. The method for producing a anti-scour radiation heat-shielding coating for titanium alloy according to claim 29, comprising the steps of:
1) The construction of the primer layer of the bonding layer comprises the following steps: firstly, carrying out sand blasting treatment on the titanium alloy to remove an oxide layer, carrying out air spraying on the primer of the bonding layer, adjusting viscosity before spraying, drying the surface of the primer after finishing spraying, and heating and curing to obtain a primer coating;
2) The construction of the high emissivity layer comprises the following steps: and (3) on the basis of the primer coating in the step (1), carrying out air spraying on the high-emissivity coating, uniformly mixing the component A and the component B before spraying, regulating the viscosity, carrying out surface drying on the sprayed coating, and heating and curing to obtain a high-emissivity layer.
31. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
in the construction of the primer layer of the bonding layer in the step 1),
the viscosity is adjusted to 10-30 s by adopting a diluent before spraying.
32. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
in the construction of the primer layer of the bonding layer in the step 1),
the air spraying is carried out by adopting a small-caliber spray gun; wherein the caliber of the small caliber spray gun is 0.3-1.2 mm.
33. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
in the construction of the primer layer of the bonding layer in the step 1),
the surface drying temperature is room temperature, and the drying time is 1-4 hours;
the conditions for heat curing include: the temperature is 120-150 ℃ and the time is 30-90 min.
34. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 31, wherein:
the viscosity is adjusted to be 12-20 s by adopting a diluent before spraying.
35. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 32, wherein:
the caliber of the small-caliber spray gun is 0.5-0.8 mm.
36. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
in the construction of the high emissivity layer in the step 2),
the viscosity is adjusted to 15-40 s by adopting a diluent.
37. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
in the construction of the high emissivity layer in the step 2),
the air spraying is carried out by adopting a spray gun; the caliber of the spray gun is 0.5-0.8 mm.
38. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
in the construction of the high emissivity layer in the step 2),
the surface drying temperature is room temperature, and the drying time is 1-4 hours;
the conditions for heat curing include: the temperature is 180-200 ℃ and the time is 2-4 hours.
39. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 36, wherein:
the viscosity is adjusted to 20-30 s by adopting a diluent.
40. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
the preparation method of the bonding layer primer comprises the following steps:
and (3) blending and dispersing the components including the polysilazane and the high-temperature-resistant filler.
41. The method for producing a titanium alloy anti-scour radiation heat-shielding coating according to claim 30, wherein:
the preparation method of the component A of the high-emissivity coating comprises the following steps:
and grinding and blending the components comprising the high-temperature resistant resin solution, the high-emissivity filler and the high-temperature resistant filler.
42. The method for preparing a anti-scour radiation heat-insulating coating for a titanium alloy according to claim 40, wherein:
in the preparation method of the bonding layer primer,
the blending is carried out at a high speed, and the stirring speed is 1000-3000 rpm.
43. The method for preparing a anti-scour radiation heat-insulating coating for a titanium alloy according to claim 41, wherein:
in the preparation method of the component A of the high-emissivity coating,
the grinding and blending adopts 2mm zirconium beads and 1mm zirconium beads as grinding media, and the grinding rotating speed is 1000-3000 rpm.
44. Use of a titanium alloy of any one of claims 1 to 28 in a scour radiation heat barrier coating or a coating prepared according to the method of any one of claims 29 to 43 in high speed aircraft, weapons.
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