CN110117765B - TiO 2 2 Base electrothermal coating and preparation method thereof - Google Patents
TiO 2 2 Base electrothermal coating and preparation method thereof Download PDFInfo
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- CN110117765B CN110117765B CN201910413283.5A CN201910413283A CN110117765B CN 110117765 B CN110117765 B CN 110117765B CN 201910413283 A CN201910413283 A CN 201910413283A CN 110117765 B CN110117765 B CN 110117765B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/073—Metallic material containing MCrAl or MCrAlY alloys, where M is nickel, cobalt or iron, with or without non-metal elements
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/08—Metallic material containing only metal elements
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/18—After-treatment
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/03—Electrodes
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
Abstract
The invention discloses a TiO 2 2 The electrothermal coating coated on the surface of a substrate sequentially comprises a bonding layer, an insulating and heat-insulating layer, a ceramic heating layer and an insulating and heat-conducting protective layer from bottom to top, and is connected with a power supply through electrodes embedded at two ends of the ceramic heating layer and binding posts on the electrodes. The ceramic heating coating material is TiO 2 Based on a ceramic material, the dopant comprising Al 2 O 3 ，MgAl 2 O 4 ，Cr 2 O 3 And at least one of YSZ, and the control of the resistance value and the heating effect is realized by regulating and controlling the thickness of the coating, the dopant material and the proportion. The electrothermal coating layers are well combined, the tissue is uniform and compact, the heating speed is high, the temperature distribution is uniform, and the long-time stable operation at the temperature below 350 ℃ can be met under the condition of low energy consumption; the preparation method has high efficiency and low cost, and the preparation process is environment-friendly and pollution-free.
Description
Technical Field
The invention relates to the technical field of heating, in particular to TiO 2 A base electrothermal coating and a preparation method thereof.
Background
The electric heating device is widely applied to various fields of national production and life and national defense construction. The traditional electric heating mode mainly adopts the electric heating wire arranged on the inner side of the substrate as a heating body, and the heat generated by the electric heating wire is transferred to the outer surface through the base material, so the problems of complex structure, uneven temperature distribution, low energy utilization rate, high cost, short service life and the like generally exist. In addition, in order to maintain a certain temperature on the surface of the substrate, the internal temperature is inevitably overhigh and the temperature difference between the inside and the outside of the material is relatively large, which puts forward higher temperature-resistant requirements on the material.
In recent years, a method of obtaining a uniform temperature distribution by directly applying an electrothermal coating layer on the surface of a substrate as a heating element instead of an electric heating wire has been attracting attention. The thermal spraying is an economic and efficient coating preparation means, can be used for preparing a thin and uniform heating element on the surface of a substrate, and directly generates uniform radiant heat on the surface after being electrified, thereby realizing the heating function. The heating coatings prepared by the thermal spraying method have been applied to hot air and hot water pipelines, copying and printing equipment, household plane heaters, aircraft anti-icing coatings, antibacterial coatings and the like.
The current heating layer mainly comprises metal materials such as Ni, NiCr, NiAl, NiCrAlY or FeCrAlY. However, the metal coating needs to have a complicated geometric shape (such as a coil, a bent pipe and the like) and a low thickness to achieve the required resistance, and resistance variation or local oxidation and other phenomena in the use process can cause uneven resistance and local over-temperature, so that the service life of the metal coating is influenced, and the application of the metal material electric heating coating facing higher service temperature is restricted.
The ceramic conductive coating has the characteristics of higher resistivity, insensitivity to oxidation, better matching of thermal expansion coefficient with an insulating and heat-insulating layer, high hardness, good wear resistance and corrosion resistance, stable chemical property, difficult oxidation and the like, and is an ideal material for an electrothermal coating at a higher service temperature. Common conductive ceramic materials include titanium dioxide (TiO) 2 ) Molybdenum disilicide (MoSi) 2 ) Silicon carbide (SiC), zinc oxide (ZrO), and the like. Wherein, TiO 2 As a semiconductor ceramic, the dielectric constant is between that of a conductive ceramic and that of an insulating ceramic, and the electrical conductivity rapidly increases with increasing temperature; in the preparation process, TiO 2 The powder can generate a small amount of oxygen loss under high temperature and reducing atmosphere to become titanium oxide in an oxygen-deficient state, a large amount of oxygen holes and free electrons are formed, and the conductivity of the powder is obviously increased. Thus, TiO 2 Is an alternative material for the heat coat.
For example, Chinese patent CN101588656B, which provides a TiO for heating roller 2 A base ceramic heating coating and a preparation method thereof. Al-containing coating prepared by atmospheric plasma spraying 2 O 3 TiO of dopant 2 The base heating coating can stably work above 300 ℃. But TiO prepared in atmospheric environment 2 In the base electric heating coating, the content of the conductive main component anoxic phase is limited, the coating has inherent characteristics of high porosity and the like, and the coating is subject to failure due to rapid increase of resistivity, uneven local heating and the like in the service process. Therefore, there is a need to develop an electrothermal coating with a more uniform and dense texture structure and a higher content of oxygen-deficient phase, and which can be stably used at higher temperature.
Disclosure of Invention
The invention aims to solve the problems of uneven heating, short service life and the like caused by the traditional resistance wire or metal electric heating coating, and obtain the electric heating coating which has more uniform and compact tissue structure, higher anoxic phase content and can be stably in service at higher temperature.
In order to achieve the above object, the present invention is achieved by the following means.
The invention provides a TiO 2 The base electric heating coating is coated on the surface of a matrix and sequentially comprises a bonding layer, an insulating thermal insulation layer, a ceramic heating layer and an insulating heat conduction protective layer from bottom to top, electrodes embedded at two ends of the ceramic heating coating and wiring posts on the electrodes, and the preparation material of the ceramic heating layer comprises TiO 2 Radical-doped oxides. The tie coat sets up in the surface of base member, and insulating thermal insulation layer sets up in the surface of tie coat, and the ceramic heating layer sets up in insulating thermal insulation layer's surface, and insulating heat conduction inoxidizing coating sets up in the surface of ceramic heating layer. The coated electric heating coating is connected with a power supply through electrodes embedded at two ends of the ceramic heating layer and binding posts on the electrodes. The coating layers are well combined, the tissue is uniform and compact, the heating speed is high, the temperature distribution is uniform, and the long-term stable operation at the temperature below 350 ℃ can be met under the condition of low energy consumption;
Preferably, the thickness of the bonding layer is 80-200 μm, the thickness of the insulating and heat-insulating layer is 150-300 μm, the thickness of the ceramic heating layer is 200-500 μm, and the thickness of the insulating and heat-conducting protective layer is 80-300 μm;
preferably, the material of the bond coat comprises at least one of NiAl, NiCr, NiCrAlY, CoCrAlY, NiCoCrAlY or CoNiCrAlY. The bonding layer is used as a transition layer between the ceramic surface layer and the substrate, and is mainly used for reducing the thermal stress between the ceramic surface layer and the substrate caused by the mismatching of thermal expansion coefficients, enhancing the bonding strength of the coating and the substrate and ensuring the long-term service stability of the coating at a higher temperature. In addition, the oxidation and corrosion resistance of the whole coating system can be improved;
preferably, the material of the insulating and heat-insulating layer comprises aluminum oxide (Al) 2 O 3 ) Magnesium aluminate spinel (MgAl) 2 O 4 ) Chromium oxide (Cr) 2 O 3 ) Or Yttria Stabilized Zirconia (YSZ). The insulating layer not only ensures the insulation between the substrate and the electric heating layer, but also plays a role in isolating the heat generated by the ceramic heating layer from being conducted to the substrate, so that the heating efficiency can be improved, and the temperature resistance requirement on the substrate material can be reduced;
preferably, the doped oxide comprises Al 2 O 3 、MgAl 2 O 4 、Cr 2 O 3 YSZ and the TiO by mechanical mixing 2 And (4) uniformly mixing. The ceramic conductive coating is an ideal material for the heating coating because of the advantages of higher resistivity, insensitivity to oxidation, better matching of thermal expansion coefficient with the insulating and heat-insulating layer and the like. And TiO 2 2 As a semiconductor ceramic, the dielectric constant is between conductive ceramic and insulating ceramic, the conductivity is rapidly increased along with the increase of temperature, the semiconductor ceramic has the advantages of stable chemical characteristics, good heat resistance, high oxidation resistance, strong corrosion resistance and the like, and also has higher infrared radiation and far infrared radiation rate, far infrared waves can be radiated when the semiconductor ceramic is heated, the energy of the wavelength is easily absorbed by the molecules of high molecular organic substances (such as paint), water, air and the like, the violent vibration and rotation of the molecules and atoms are caused, the resonance phenomenon is generated, and the internal heat is generated, so the internal drying process of the substances is accelerated, and the aims of shortening the heating time, improving the heating efficiency, saving energy and saving electricity are fulfilled. Thus, TiO 2 Is suitable for being applied in a heating coating system; and by doping oxides with TiO 2 The composite material is formed, and the microstructure and the resistance of the coating can be regulated and controlled to improve the oxidation resistance and the electric heating performance of the coating;
Preferably, the doped oxide is the same as the material of the insulating thermal barrier coating. The dopant in the ceramic heating layer is made of the same material as the insulating heat-insulating coating to form gradient transition with the insulating heat-insulating coating, so that the thermal stress between the electric heating coating and the insulating heat-insulating coating caused by the difference of thermal expansion coefficients in the coating preparation and subsequent service heating processes can be reduced, and the bonding strength of the electric heating coating and the insulating heat-insulating coating is improved;
preferably, the content of the doped oxide is 10 to 50 wt%. The control of the resistance value and the heating effect can be realized by regulating and controlling the thickness of the heating layer, the variety and the proportion of dopant materials;
preferably, the insulating and heat-conducting protective layer material comprises aluminum oxide-aluminum nitride (Al) 2 O 3 AlN) of Al 2 O 3 Is used as a main component, is doped with AlN with certain content, and is subjected to spray granulation to obtain composite powder suitable for a spray coating process. In the service process, the surface of the electric heating coating can be in direct contact with a workpiece, and in order to isolate the electrical contact between the workpiece and the roller body, the surface of the coating needs to be subjected to insulation treatment. Furthermore, TiO 2 If the oxygen-deficient phase in the base heating layer is directly exposed to the air environment, oxidation may occur to convert the phase back to the rutile phase, thereby reducing the heating efficiency. Therefore, the protective layer coated on the surface of the heating layer can isolate the workpiece from being in electrical contact with the heating layer and also isolate the heating layer from being in direct contact with the atmosphere so as to weaken the oxidation process of the workpiece. In addition, in order to ensure the heating efficiency, the protective layer also has good heat-conducting property. And Al 2 O 3 The material has the properties of high hardness, oxidation resistance, corrosion resistance, high electrical insulation and the like; AlN has excellent thermal conductivity, good electrical insulation and stable chemical properties. The composite material formed by mixing the two materials has excellent comprehensive properties of insulation and heat conduction, can provide good wear-resistant and corrosion-resistant protection, and can meet the protection requirement in the service process of an electric heating coating;
preferably, the electrode is made of a material comprising industrially pure copper. The adopted industrial pure copper has good conductivity and corrosion resistance.
The invention also provides TiO 2 A method for preparing a base electrothermal coating, the method comprising the steps of:
(1) degreasing, sandblasting and coarsening the matrix, and preheating the matrix;
(2) sequentially spraying a bonding layer, an insulating thermal-insulating layer, a ceramic heating layer and an insulating heat-conducting protective layer on the surface of the substrate;
(3) carrying out heat treatment in a hydrogen reducing atmosphere, and then grinding and polishing;
(4) electrodes and binding posts are embedded at two ends of the ceramic heating layer.
Preferably, the non-spraying part is protected after degreasing and degreasing in the step (1), sand blasting coarsening is carried out until the surface roughness Ra is more than 3 μm, the matrix coarsened by sand blasting is arranged at a position vertical to a spray gun, and the matrix is subjected to preheating treatment by using spray gun jet flow under the condition of no powder feeding. The sand blasting process can remove impurities and oxide scales on the surface of the substrate so as to increase the bonding strength between the coating and the substrate. It is worth to be noted that degreasing, sand blasting, coarsening and preheating treatment adopted in the application are all general techniques in the technical field, and specific treatment parameters are not limited by the invention;
Preferably, the ceramic heating layer is sprayed in the step (2) by using a low-pressure plasma spraying method; most preferably, the spraying conditions are: the spraying chamber is vacuumized to be below 100Pa, then protective atmosphere is filled in to ensure that the pressure in the spraying chamber is 4-60kPa, the current of a plasma spray gun is 550-700A, the argon is 40-50L/min, the hydrogen is 8-14L/min, the spraying distance is 150-300mm, and the gun moving speed is 200-1000 mm/s. The porosity of the prepared ceramic heating layer is less than 2%. The plasma jet expands rapidly at a lower atmospheric pressure in the spray chamber, and although the energy density is reduced compared with that at normal pressure, the molten TiO flying at the center of the plasma jet 2 The particles are more prone to oxygen loss and change into the anoxic Ti in the high-temperature jet flow with low oxygen partial pressure 2 O 3 、 Ti 3 O 5 And Magneli phase (Ti) n O 2n-1 N is more than or equal to 4 and less than or equal to 10), high reducibility H in plasma reaction gas 2 And the generation of an oxygen-deficient phase in the coating can be promoted, so that a large number of oxygen holes and free electrons are formed, and the improvement of the conductivity of the coating is facilitated. Meanwhile, the coating prepared by the low-pressure plasma spraying method has a more compact structure and fewer defects, and the impedance among particles is lower than that of the coating obtained by atmospheric plasma spraying, so that the TiO sprayed by the low-pressure plasma is coated 2 The base coating has higher conductivity, even can reach more than several times of the atmospheric plasma spraying coating. In addition, the uniform and compact coating structure can also reduce the local heating unevenness in the service processRisk of rapid failure. The preparation processes of the bonding layer and the insulating layer are mature, so that the spraying method and specific parameters are not limited;
preferably, the step (2) is performed by at least one of atmospheric plasma spraying or low-pressure plasma spraying. Most preferably, the spraying conditions are: vacuumizing the spraying chamber to be below 100Pa, then filling protective atmosphere to ensure that the pressure in the spraying chamber is 4-60kPa, the current of a plasma spray gun is 600-700A, the argon is 38-50L/min, the hydrogen is 8-12L/min, the powder feeding speed is 20-40g/min, the spray distance is 150-300mm, and the gun moving speed is 200-1000 mm/s. By adopting a low-pressure plasma spraying method, a more compact coating structure can be obtained so as to ensure that the coating meets the insulation requirement under a thinner thickness and has excellent heat-conducting property;
preferably, the specific conditions of the heat treatment in the step (3) are as follows: and (3) placing the substrate coated with the electrothermal coating in the step (2) in a hydrogen reducing atmosphere furnace, carrying out heat treatment at the temperature of 400-900 ℃ for 1-10h, and then cooling the furnace to room temperature. At a suitable temperature, the following reaction may occur: 2TiO 2 2 +H 2 →Ti 2 O 3 +H 2 And O. Therefore, the heat treatment in a hydrogen reducing atmosphere can further improve TiO 2 The content of the anoxic phase in the coating is heated, and the thermal stress generated in the coating preparation process is released. It is worth mentioning that if the heat treatment temperature is too low, the reduction effect is not obvious or the required heat treatment time is too long; if the heat treatment temperature is too high, although it is advantageous to improve the reduction effect and shorten the heat treatment time, it may also cause deformation of the substrate and peeling of the coating due to the difference in thermal expansion coefficient between the coatings.
In addition, the ceramic heating coating which is oxidized after being used for a long time can be subjected to hydrogen reducing atmosphere heat treatment again to recover the heating effect without thoroughly removing the coating and spraying again, so that the operation cost of related equipment is reduced;
preferably, the grinding and polishing in step (3) is specifically: after the heat treatment is finished, grinding and polishing the surface of the insulating heat-conducting protective layer and the positions of the connecting electrodes at the two ends of the ceramic heating layer until the surface roughness Ra is less than 0.8 mu m; most preferably, Ra < 0.2 μm. So that the surface of the coating is uniform and smooth, the contact between the ceramic heating layer and the electrodes is increased, and a workpiece to be heated is not scratched when the ceramic heating layer is used;
Preferably, the step (4) is specifically: electrodes and mounting binding posts are embedded at two ends of the ceramic heating layer, and a gap between the electrodes and the ceramic heating layer is filled with high-temperature conductive silver adhesive so as to ensure that the connection between a power supply and the electric heating coating is effectively smooth.
The TiO provided by the invention 2 Compared with the prior art, the base electrothermal coating and the preparation method thereof have the following beneficial effects:
(1) the electrothermal coating is uniformly distributed on the outer surface of the substrate, a complex shape is not needed, heat can be directly generated on the surface of the substrate, most of the heat generated by the ceramic heating layer is transferred outwards to heat a workpiece under the action of the insulating heat-insulating coating at the lower part of the ceramic heating layer, the heating uniformity can be obviously improved, the energy consumption of the system is reduced, the heating efficiency is improved, the temperature resistance requirement on the substrate material is reduced, and the defects of nonuniform heating, short service life and the like caused by the traditional resistance wire or metal electrothermal coating are obviously overcome;
(2) TiO prepared by low-pressure plasma spraying method 2 The structure of the base ceramic heating layer is uniform and compact, the defects such as pores, cracks and the like are few, and the content of anoxic phases in the ceramic heating layer is high under the low-oxygen and high-reduction atmosphere; and through heat treatment in a hydrogen reducing atmosphere, the content of an anoxic phase in the ceramic heating layer can be further improved, stress generated in the coating preparation process is released, and the heating uniformity and the service stability are favorably improved. The TiO provided by the invention 2 The combination of all coatings of the base electric heating coating is good, and the long-term stable operation at the temperature below 350 ℃ can be met under the condition of low energy consumption;
(3) the insulating heat-conducting protective layer is sprayed by low-pressure plasma, so that the porosity of the coating can be effectively reduced, the heat conduction efficiency and the insulating effect are improved, gas-liquid erosion channels can be reduced to improve the corrosion resistance of the electrothermal coating, the insulating heat-conducting protective layer also has excellent wear resistance, and the durability of the coating can be improved;
(4) the preparation method has high efficiency, low cost, environment-friendly preparation process and no pollution. The ceramic heating coating which is oxidized after being used for a long time can be subjected to reduction heat treatment again to recover the heating effect, so that the running cost of the electric heating coating can be effectively reduced;
(5) the electrothermal coating and the preparation method thereof provided by the invention are also suitable for coating on a roller-shaped substrate to manufacture an electrothermal roller, and can be used for replacing the traditional oil (water or steam) guide heating roller and an electromagnetic induction heating roller.
Drawings
FIG. 1 shows TiO of the present invention 2 A flow chart of the preparation of the base electrothermal coating;
FIG. 2 shows TiO of the present invention 2 A schematic structure diagram of the base electrothermal coating;
FIG. 3 shows TiO of the present invention 2 The cross-sectional structure schematic diagram of the base electrothermal coating;
wherein: 1-a substrate; 2-a tie layer; 3-insulating and heat-insulating layer; 4-a ceramic heating layer; 5-insulating heat-conducting protective layer; 6-an electrode; 7-terminal.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The technical scheme of the invention is further explained in detail by combining the attached drawings.
Example 1
TiO 2 2 The preparation method of the base electrothermal coating is shown in figure 1 and specifically comprises the following steps:
(1) degreasing and deoiling a matrix, sandblasting and coarsening the matrix until the surface roughness Ra is more than 3 mu m, preheating the matrix, and spraying a NiCr bonding layer with the thickness of 100 mu m and MgAl with the thickness of 200 mu m in sequence 2 O 4 An insulating and heat-insulating layer;
(2) at MgAl 2 O 4 And a ceramic heating layer is prepared on the surface of the insulating layer. The ceramic heating layer is made of TiO 2 -40wt％MgAl 2 O 4 . Wherein, TiO 2 The particle size is 15-45 mu m, MgAl 2 O 4 The particle size is 10-45 μm. Vacuumizing the spraying chamber to be below 100Pa, then filling protective atmosphere to ensure that the pressure in the spraying chamber is 6kPa, the current of a plasma spray gun is 600A, the argon gas is 45L/min, the hydrogen gas is 12L/min, the spraying distance is 270mm, the gun moving speed is 400mm/s, and a ceramic heating layer with the thickness of 320 mu m is obtained;
(3) Preparing Al on the surface of ceramic heating layer 2 O 3 An AlN insulating heat-conducting protective layer with the powder granularity of 22-45 mu m, vacuumizing a spraying chamber to be below 100Pa, filling protective atmosphere to ensure that the pressure in the spraying chamber is 6kPa, the current of a plasma spray gun is 630A, the argon gas is 44L/min, the hydrogen gas is 11L/min, the spraying distance is 270mm, the gun moving speed is 400mm/s, and obtaining Al with the thickness of 220 mu m 2 O 3 -an AlN insulating and thermally conductive protective layer;
(4) placing the substrate coated with the electrothermal coating system in a hydrogen reducing atmosphere furnace, carrying out heat treatment for 2 hours at 800 ℃, and cooling the furnace to room temperature;
(5) grinding and polishing the two ends of the ceramic heating coating and the surface of the insulating heat-conducting protective layer until the roughness Ra is less than 0.2 mu m, wherein the total thickness of the processed coating is 720 mu m. Electrodes and binding posts are embedded at two ends of the ceramic heating layer, and a gap between the ceramic heating layer and the electrodes and the binding posts is filled by high-temperature conductive silver adhesive.
FIGS. 2 and 3 show TiO of the present invention, respectively 2 The structure schematic diagram and the section structure schematic diagram of the base electrothermal coating.
Example 2
TiO 2 2 The preparation method of the base electrothermal coating comprises the following steps:
(1) degreasing and deoiling a matrix, sandblasting and coarsening the matrix until the surface roughness Ra is more than 3 mu m, preheating, and spraying a NiAl bonding layer with the thickness of 120 mu m and Al with the thickness of 250 mu m in sequence 2 O 3 An insulating and heat-insulating layer;
(2) in Al 2 O 3 And a ceramic heating layer is prepared on the surface of the insulating layer. The ceramic heating layer is made of TiO 2 -30wt％Al 2 O 3 . Wherein, TiO 2 Grain size of 15-45 μm, Al 2 O 3 The particle size is 5-22 μm. Vacuumizing the spraying chamber to be below 100Pa, then filling protective atmosphere to ensure that the pressure in the spraying chamber is 13kPa, the current of a plasma spray gun is 620A, the argon gas is 42L/min, the hydrogen gas is 10L/min, the spraying distance is 240mm, the gun moving speed is 300mm/s, and obtaining a ceramic heating layer with the thickness of 350 mu m;
(3) preparing Al on the surface of a ceramic heating layer 2 O 3 An AlN insulating heat-conducting protective layer with the powder granularity of 15-45 mu m, vacuumizing a spraying chamber to be below 100Pa, filling protective atmosphere to ensure that the pressure in the spraying chamber is 13kPa, the current of a plasma spray gun is 650A, the argon is 42L/min, the hydrogen is 10L/min, the spraying distance is 240mm, the gun moving speed is 300mm/s, and obtaining the Al with the thickness of 200 mu m 2 O 3 -an AlN insulating and thermally conductive protective layer;
(4) placing the substrate coated with the electrothermal coating system in a hydrogen reducing atmosphere furnace, carrying out heat treatment for 4 hours at 700 ℃, and cooling the furnace to room temperature;
(5) and grinding and polishing the two ends of the ceramic heating coating and the surface of the insulating heat-conducting protective layer until the roughness Ra is 0.4 mu m, and the total thickness of the processed coating is 850 mu m. Electrodes and binding posts are embedded at two ends of the ceramic heating layer, and a gap between the ceramic heating layer and the electrodes and the binding posts is filled by high-temperature conductive silver adhesive.
Example 3
TiO 2 2 The preparation method of the base electrothermal coating comprises the following steps:
(1) degreasing and deoiling a matrix, sandblasting and coarsening the matrix until the surface roughness Ra is more than 3 mu m, preheating, and sequentially spraying a NiCrAlY bonding layer with the thickness of 90 mu m and a YSZ insulating and heat-insulating layer with the thickness of 180 mu m;
(2) and preparing a ceramic heating layer on the surface of the YSZ insulating and heat-insulating layer. The ceramic heating layer is made of TiO 2 -45 wt% YSZ. Wherein, TiO 2 The granularity is 10-45 μm, and the YSZ granularity is 22-45 μm. Vacuumizing the spraying chamber to be below 100Pa, then filling protective atmosphere to ensure that the pressure in the spraying chamber is 30kPa, the current of a plasma spray gun is 650A, the argon gas is 42L/min, the hydrogen gas is 9L/min, the spraying distance is 180mm, the gun moving speed is 500mm/s, and the ceramic heating layer with the thickness of 260 mu m is obtained;
(3) preparing Al on the surface of a ceramic heating layer 2 O 3 An AlN insulating heat-conducting protective layer with the powder granularity of 15-53 mu m, vacuumizing a spraying chamber to be below 100Pa, filling protective atmosphere to ensure that the pressure in the spraying chamber is 30kPa, the current of a plasma spray gun is 660A, the argon is 46L/min, the hydrogen is 9L/min, the spraying distance is 180mm, the gun moving speed is 500mm/s, and obtaining the Al with the thickness of 180 mu m 2 O 3 -an AlN insulating and thermally conductive protective layer;
(4) placing the substrate coated with the electrothermal coating system in a hydrogen reducing atmosphere furnace, carrying out heat treatment for 6 hours at 600 ℃, and cooling the furnace to room temperature;
(5) And grinding and polishing the two ends of the ceramic heating coating and the surface of the insulating heat-conducting protective layer until the roughness Ra is 0.3 mu m, and the total thickness of the processed coating is 620 mu m. Electrodes and binding posts are embedded at two ends of the ceramic heating layer, and a gap between the ceramic heating layer and the electrodes and the binding posts is filled by high-temperature conductive silver adhesive.
Example 4
TiO (titanium dioxide) 2 The preparation method of the base electrothermal coating comprises the following steps:
(1) degreasing and deoiling a matrix, sandblasting and coarsening the matrix until the surface roughness Ra is more than 3 mu m, preheating, and sequentially spraying a CoNiCrAlY bonding layer with the thickness of 130 mu m and Cr with the thickness of 220 mu m 2 O 3 An insulating and heat-insulating layer;
(2) in Cr 2 O 3 And a ceramic heating layer is prepared on the surface of the insulating layer. The ceramic heating layer is made of TiO 2 -25wt％Al 2 O 3 . Wherein, TiO 2 Grain size of 10-45 μm, Cr 2 O 3 The particle size is 20-45 μm. Vacuumizing the spraying chamber to be below 100Pa, then filling protective atmosphere to ensure that the pressure in the spraying chamber is 45kPa, the current of a plasma spray gun is 660A, the argon gas is 48L/min, the hydrogen gas is 9L/min, the spraying distance is 150mm, the gun moving speed is 700mm/s, and obtaining a ceramic heating layer with the thickness of 330 mu m;
(3) preparing Al on the surface of a ceramic heating layer 2 O 3 AlN insulating heat-conducting protective layer with a powder particle size of 10-40 μm, an atmosphere plasma torch current of 660A, argon gas 40L/min, hydrogen gas 11L/min, a spray distance of 110mm, a torch speed of 45mm/s, and a thickness of the resultant Al with a thickness of 240 μm 2 O 3 -an insulating and thermally conductive protective layer of AlN;
(4) placing the substrate coated with the electrothermal coating system in a hydrogen reducing atmosphere furnace, carrying out heat treatment for 8 hours at 500 ℃, and cooling the furnace to room temperature;
(5) grinding and polishing the two ends of the ceramic heating coating and the surface of the insulating heat-conducting protective layer until the roughness Ra is less than 0.2 mu m, and the total thickness of the processed coating is 780 mu m. Electrodes and binding posts are embedded at two ends of the ceramic heating layer, and a gap between the ceramic heating layer and the electrodes and the binding posts is filled by high-temperature conductive silver adhesive.
Verification example
The above examples 1 to 4 were repeated to obtain sufficient TiO 2 The porosity and stable heating temperature detection data of the obtained ceramic heating layer are listed in table 1. The porosity of the ceramic heating layer is obtained by quantitatively measuring a metallographic sample by adopting Image analysis software UTHSCSA Image Tool, and the surface temperature of the electrothermal coating is obtained by adopting an infrared thermometer.
TABLE 1 porosity (%) of ceramic heating layer and surface-stabilized heating temperature (. degree. C.) of electrothermal coating
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Porosity (%) | 0.9 | 1.3 | 1.1 | 1.2 |
| Temperature of Stable heating (. degree.C.) | 360 | 345 | 348 | 320 |
As can be seen from Table 1, the heating coating has a relatively suitable porosity and stable heating temperatures of above 300 ℃.
In conclusion, the electrothermal coating directly prepared on the surface of the substrate has uniform and compact structure, uniform heating and low energy consumption, and can stably run for a long time at the temperature of below 350 ℃. The preparation method has high efficiency, low cost, environment-friendly preparation process and no pollution.
The above detailed description section specifically describes the analysis method according to the present invention. It should be noted that the above description is only for the purpose of helping those skilled in the art better understand the method and idea of the present invention, and not for the limitation of the related contents. The present invention may be appropriately adjusted or modified by those skilled in the art without departing from the principle of the present invention, and the adjustment and modification also fall within the scope of the present invention.
Claims (10)
1. TiO 2 2 The electric heating coating comprises a bonding layer, an insulating and heat-insulating layer, a ceramic heating layer, an insulating and heat-conducting protective layer, electrodes embedded at two ends of the ceramic heating layer and binding posts arranged on the electrodes, wherein the bonding layer, the insulating and heat-insulating layer, the ceramic heating layer and the binding posts are sequentially arranged on the substrate surface from bottom to top, and a preparation material of the ceramic heating layer comprises TiO 2 A radical-doped oxide;
The thickness of the ceramic heating layer is 200-500 mu m; the doped oxide comprises Al 2 O 3 、MgAl 2 O 4 、Cr 2 O 3 And YSZ, the content of the doped oxide is 10-50 wt%.
2. The TiO of claim 1 2 A base electrothermal coating, characterized in that the material of the bonding layer comprises at least one of NiAl, NiCr, NiCrAlY, CoCrAlY, NiCoCrAlY or CoNiCrAlY, the thickness of the bonding layer being 80-200 μm.
3. The TiO of claim 1 2 The base electrothermal coating is characterized in that the material of the insulating and heat-insulating layer comprises Al 2 O 3 、MgAl 2 O 4 、Cr 2 O 3 And YSZ, the thickness of the insulating and heat-insulating layer is 150-300 μm.
4. The TiO of claim 1 2 The base electric heating coating is characterized in that the insulating heat-conducting protective layer material comprises aluminum oxide-aluminum nitride, and the thickness of the insulating heat-conducting protective layer is 80-300 mu m.
5. A process for preparing the TiO of any one of claims 1 to 4 2 A method of base electro thermal coating, characterized in that the method comprises the steps of:
(1) degreasing, deoiling, sandblasting, coarsening and preheating the matrix;
(2) spraying a bonding layer, an insulating thermal-protective layer, a ceramic heating layer and an insulating heat-conducting protective layer on the surface of the substrate in sequence, wherein the ceramic heating layer comprises TiO 2 Prepared by spraying a preparation material based on a doped oxide, wherein the doped oxide comprises Al 2 O 3 、MgAl 2 O 4 、Cr 2 O 3 And YSZ, the content of the doped oxide is 10-50 wt%;
(3) carrying out heat treatment in a hydrogen reducing atmosphere, and then grinding and polishing;
(4) electrodes and binding posts are embedded at two ends of the ceramic heating layer.
6. The method according to claim 5, wherein the step (2) is carried out by spraying the ceramic heating layer by using a low-pressure plasma spraying method; the spraying conditions are as follows: the spraying chamber is vacuumized to be below 100Pa, then protective atmosphere is filled in to ensure that the pressure in the spraying chamber is 4-60kPa, the current of a plasma spray gun is 550-700A, the argon is 40-50L/min, the hydrogen is 8-14L/min, the spraying distance is 150-300mm, and the gun moving speed is 200-1000 mm/s.
7. The method of claim 5, wherein the step (2) comprises at least one of atmospheric plasma spraying or low-pressure plasma spraying.
8. The method according to claim 5, wherein the heat treatment in the step (3) is carried out under the following specific conditions: and (3) placing the substrate coated with the electrothermal coating in the step (2) in a hydrogen reducing atmosphere furnace, carrying out heat treatment at the temperature of 400-900 ℃ for 1-10h, and then cooling the furnace to room temperature.
9. The method according to claim 5, wherein the grinding and polishing process in the step (3) is specifically: and after the heat treatment is finished, grinding and polishing the surface of the insulating heat-conducting protective layer and the positions of the connecting electrodes at the two ends of the ceramic heating layer until the surface roughness Ra is less than 0.8 mu m.
10. The method according to claim 9, characterized in that the surface roughness Ra < 0.2 μ ι η.
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| CN112029410B (en) * | 2020-08-28 | 2021-10-15 | 中国航发北京航空材料研究院 | Resin-based composite material surface resistance heating coating and preparation method thereof |
| CN113957375B (en) * | 2020-11-17 | 2024-04-09 | 天津航空机电有限公司 | Structure for realizing substrate heating function and preparation method |
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