CN107400846B - Preparation method of graphene modified temperature indicating thermal barrier coating - Google Patents
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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
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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
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Abstract
The invention provides a preparation method of a graphene modified temperature indicating thermal barrier coating, which comprises the following steps: step 1: dissolving zirconium oxide octahydrate in deionized water; step 2: dissolving yttrium oxide, europium oxide and neodymium oxide solid powder in dilute hydrochloric acid; and step 3: dispersing graphene oxide in absolute ethyl alcohol; and 4, step 4: mixing the two solutions obtained in the step 2 and the step 3; and 5: stirring the mixed solution obtained in the step (1) and the solution obtained in the step (4) and adding a polyethylene glycol dispersant; step 6: preparing ammonia water reaction base solution with the pH =10, and heating the solution to obtain yttria-stabilized zirconia precursor sol; and 7: obtaining a Cl-free yttrium oxide stabilized zirconia sol of graphene modified Nd3+/Eu3 +; and 8: and spraying the graphene modified temperature-indicating thermal barrier coating by liquid-phase plasma. The invention avoids the problems of burning loss, evanescent flight and agglomeration of the nano-scale graphene in the process of preparing the coating by the thermal spraying technology.
Description
Technical Field
The invention belongs to the technical field of preparation processes of graphene modified rare earth fluorescent particle composite yttrium oxide stabilized zirconia precursor solutions, design of graphene modified temperature indicating thermal barrier coatings and processes for preparing coatings by liquid material plasma spraying, and particularly relates to a preparation method of a graphene modified temperature indicating thermal barrier coating.
Background
Currently, thermal barrier coating systems that are widely used on aircraft engines consist of an alloy substrate, an MCrAlY or Pt modified aluminide bond coat, a Thermally Grown Oxide (TGO), and a Yttria Stabilized Zirconia (YSZ) thermal barrier ceramic layer. Thermal barrier coating life prediction relies heavily on temperature measurements of the application environment. First, the surface temperature Ts of the thermal barrier coating is much higher than the surface temperature Tb of the substrate during service, and it has been reported that the temperature of the metallic bond coat increases from 1010 ℃ to 1064 ℃ and that a difference of only 54 ℃ allows the growth of TGO at a rate 3 times that of the thermal barrier coating, resulting in premature failure of the thermal barrier coating. However, the current temperature measurement methods are not sufficient for the work: on one hand, the measurement part is positioned below the ceramic surface layer of the thermal barrier coating, so that the traditional temperature measurement mode cannot be touched; on the other hand, because the internal temperature of the gas turbine is high, a series of unfavorable temperature measurement conditions such as strong electromagnetic interference, narrow space, high-speed blade operation and the like exist. Therefore, the novel thermal barrier coating with the real-time temperature response characteristic is developed, the internal rule between the service temperature and the service life of the coating is researched, and the method has important significance for effectively evaluating the service health condition of the coating and realizing the early warning failure of the thermal barrier coating.
The temperature measurement technology adopted in the high temperature environment at present mainly comprises infrared temperature measurement and thermocouple temperature measurement [6], wherein the infrared temperature measurement technology belongs to non-contact temperature measurement and has the advantages of wide temperature measurement range, no limitation of the upper limit of the temperature measurement, no damage to the temperature field of a measured object, high reaction rate and the like. However, the method has the limitation that the method is easily influenced by external factors such as the emissivity of an object, the measurement distance, smoke dust, water vapor and the like, the measurement error is large, and the influence is particularly serious in a high-temperature environment. The thermocouple is a contact temperature measurement method using thermoelectric effect, although the method has the advantages of simple operation, high reliability and high measurement precision, the temperature measurement can be realized only after reaching thermal equilibrium within a certain time because the temperature measurement element has to perform sufficient heat exchange with the measured medium, so that the delay phenomenon of temperature measurement exists, and the thermocouple is limited by high temperature resistant materials and cannot be applied to high temperature measurement.
In recent years, the fluorescence temperature measurement technology based on the optical response temperature characteristic of the material is rapidly developed, and hopes are brought to real-time monitoring of the service temperature of the thermal barrier coating and prediction of the service life of the thermal barrier coating. The principle is that rare earth fluorescent elements are doped in the thermal barrier coating, and after the thermal barrier coating is in service in different temperature environments, the spectral width, the fluorescence intensity and the fluorescence service life of a fluorescent material are correspondingly changed, so that the purpose of monitoring the service temperature of the thermal barrier coating in real time can be realized by researching the relevance of the fluorescent material and the temperature.
In recent years, thermometric studies of rare earth fluorescent elements applied to thermal barrier coatings have begun to receive attention from researchers. Gentleman M9 researches the mapping relation between the fluorescence intensity of Eu3+ doped YSZ coating and the service in the temperature range of 0-1200 ℃, and provides a decay curve of the fluorescence intensity of the coating in the temperature range, thereby providing a theoretical basis for scientifically predicting the residual life of the coating. Chen X et al studied the fluorescence intensity change of YSZ powder doped with Dy3+ and plasma sprayed YSZ: Dy3+ coating, and established the mapping relationship between the fluorescence attenuation period and the service temperature of the coating at 0-1000 ℃. Pin L et al studied rare earth doped thin films prepared by sol-gel deposition and confirmed the use of Tm3+ element at higher temperatures. Eldridge J I also attempts to add a small amount of rare earth to YSZ and measure the temperature change inside the coating by means of the characteristic wavelength and lifetime of fluorescence, so that the high temperature state of the coating can be monitored in real time.
In China, the research on the health condition of the thermal barrier coating in high-temperature service by adopting rare earth fluorescence intensity evaluation is still in the starting stage. The Eu3+ and Dy3+ doped SrAl2O4 coating is prepared by Zhongfeng university of Dalian maritime and the like through plasma spraying, the luminescence property of the coating is represented, and the luminescence mechanism of Eu3+ and Dy3+ in the coating is preliminarily discussed.
In conclusion, the rare earth fluorescent material is difficult to radiate weakly in the coating, and the intensity of the rare earth fluorescent material is rapidly attenuated after the rare earth fluorescent material is in service in a high-temperature environment for a long time. The research idea of the project is to co-dope and modify the existing rare earth elements at first so as to realize the purpose of multiplying the radiation intensity. At present, Eu3+ is used as a fluorescent doping element of a thermal barrier coating for more research, and is proved to have better light response temperature characteristics in a high-temperature environment. In addition, the double-activator doped rare earth functional material has attracted attention in recent years for enhancing the intensity of fluorescence radiation, and studies have shown that Nd3+ has energy transfer to Eu3+ and the energy transfer rate becomes large with the increase of temperature, and if it is co-doped, a wide range response of fluorescence intensity variation with temperature can be realized. In addition, Graphene Oxide (GO) is a derivative of graphene, the surface of which contains a large number of oxygen-containing functional groups, and the principle that graphene has fluorescence characteristics is caused by pi-orbital defect generation caused by the oxygen-containing functional groups generated in the graphene oxidation process. Studies have also shown that GO surface oxygen-containing functional groups affect changes in fluorescence intensity as well as position. In conclusion, the difficult problem of weak fluorescence intensity of single Eu3+ applied to thermal barrier coatings can be solved by adopting the component regulation and preparation of the graphene modified Tb3+/Eu3 +.
Accordingly, the prior art is deficient and needs improvement.
Disclosure of Invention
The invention provides a graphene modified temperature indicating thermal barrier coating and a preparation method thereof. The temperature of the coating in the whole life cycle is expected to be monitored in real time, the aim of early warning the failure of the coating is fulfilled, and a theoretical basis is laid for establishing an accurate life prediction model.
The invention aims to solve the technical problem of the prior art and provides a preparation method of a graphene modified temperature indicating thermal barrier coating.
The technical scheme of the invention is as follows:
a preparation method of a graphene modified temperature-indicating thermal barrier coating comprises the following steps:
step 1: weighing a certain amount of zirconium oxide octahydrate (ZrOCl)2·8H2O) dissolving in deionized water, and stirring and mixing;
step 2: weighing a certain amount of yttrium oxide (Y)2O3) Europium oxide (Eu)2O3) And neodymium oxide (Nd)2O3) Dissolving solid powder in 1mol/L dilute hydrochloric acid, and stirring and mixing;
and step 3: weighing a certain amount of graphene oxide, dispersing the graphene oxide in absolute ethyl alcohol, and performing ultrasonic oscillation to prepare a graphene oxide dispersion liquid;
and 4, step 4: mixing the two solutions obtained in the step 2 and the step 3, and stirring for a certain time at a certain rotating speed within a certain temperature range under a vacuum condition until the solution is in a uniform suspension state;
and 5: mixing the mixed solution of zirconium oxide octahydrate obtained in the step (1) and the graphene modified Nd obtained in the step (4)3+/Eu3+Stirring and mixing the solution for a certain time, and simultaneously adding a proper amount of polyethylene glycol (PEG 2000) dispersant;
step 6: preparation of aqueous Ammonia (NH) pH =103·H2O) reaction base liquid, gradually dripping ammonia water reaction base liquid into the solution obtained in the step 5, simultaneously heating the solution to keep the constant temperature of 80 ℃, and stirring for a certain time to obtain graphene modified Nd with the pH = 3-63+/Eu3+The yttria-stabilized zirconia (YSZ) precursor sol of (a);
and 7: by using hydrogen peroxide (H)2O2) Oxidizing agent oxidation and semipermeable membrane dialysis-Removing, and titrating with silver nitrate until no white AgCl flocculent precipitate is generated to obtain Cl-free solution-Modified Nd of graphene3+/Eu3+The yttria-stabilized zirconia sol of (a);
and 8: a matrix sample used for preparing the coating is 45 steel, and the matrix is degreased by acetone, and then is subjected to conventional ultrasonic cleaning and surface sand blasting pretreatment so as to improve the roughness and the activation degree of the matrix surface. And spraying a NiCoCrAIY bonding bottom layer with the thickness less than or equal to 0.1mm on the pretreated substrate by using a traditional powder plasma spraying process, and then spraying a graphene modified temperature-indicating thermal barrier coating by using liquid-phase plasma.
In the foregoingZirconium oxide octahydrate (ZrOCl) in steps 1 and 2 above2·8H2O) and yttrium oxide (Y)2O3) The mass percentage is 28-30: 1.
In the above, europium oxide (Eu) in the step 22O3) And neodymium oxide (Nd)2O3) Mixing with dilute hydrochloric acid; wherein the mass percentage of the europium oxide and the neodymium oxide is 1.5-2: 1, and the mixture is uniformly stirred for 30-60 min by a high-speed stirrer at the speed of 500 rpm/min.
In the step 3, a certain amount of graphene oxide is dispersed in absolute ethyl alcohol and subjected to ultrasonic oscillation to prepare a graphene oxide dispersion liquid, wherein the mass percentage of the graphene oxide to the absolute ethyl alcohol is 1: 100-300, the temperature is kept at 80-100 ℃, the ultrasonic dispersion time is 120-180 min, and the ultrasonic frequency is 15 Hz.
In the step 4, the two solutions obtained in the step 2 and the step 3 are mixed, the temperature is kept at 350-400 ℃ under a vacuum condition, and the high-speed stirrer is used for uniformly stirring for 30-60 min at the speed of 500 rpm/min.
In the above step 5, the mixed solution is stirred for 60-90 min at a stirring speed of 500rmp/min, and 30-50 g of polyethylene glycol dispersant is added.
In the above, the liquid material plasma spraying process parameters for preparing the graphene modified temperature indicating thermal barrier coating in the step 8 are that the flow of argon (Ar) is 28-40L/min, the flow of hydrogen (H2) is 8-15L/min, the spraying voltage is 70-80V, the spraying current is 550-660A, the spraying distance is 80-120 mm, and the graphene modified Nd is3+/Eu3+The sol rate of the Yttria Stabilized Zirconia (YSZ) precursor is 100-150 g/min, the preheating temperature of the matrix is 500-700 ℃, and the pressure of the precursor liquid material conveying gas is 0.3-0.6 MPa.
In the above, the graphene modified temperature indicating thermal barrier coating prepared in step 8 is a gradient composite coating, the bottom layer is a NiCoCrAIY bonded bottom layer, the graphene modified temperature indicating thermal barrier coating is a surface layer, the surface layer is divided into 4 layers, the thickness of each layer is about 50-60 μm, the total thickness is about 300-350 μm, the thickness is close to that of the NiCoCrAIY bonded bottom layer and the surface layer, and the graphene mass percentage content in each graphene modified temperature indicating thermal barrier coating is respectively 2%, 1.5%, 1% and 0.5%.
Compared with the closest prior art, the invention has the following beneficial effects:
1) compared with the difficulty that the service temperature of a YSZ thermal barrier coating prepared by traditional thermal spraying cannot be known, the liquid material graphene modified europium oxide and neodymium oxide co-doped yttrium oxide stabilized zirconia precursor sol and the temperature indicating thermal barrier coating prepared by adopting the liquid material plasma spraying technology can monitor the temperature change in the full thickness range inside the thermal barrier coating in real time, can play a role in early warning the failure of the coating and can monitor the integrity and the safe service condition of the thermal barrier coating.
2) Compared with the single rare earth ion Eu3+ applied to the high temperature of the thermal barrier coating, the difficulty of weak fluorescence intensity exists, and the high-sensitivity response of the fluorescence intensity ratio can be realized in a wider temperature range for preparing the temperature-indicating thermal barrier coating through a synergistic action mechanism of Nd3+/Eu3+ co-doping.
3) According to the technical scheme provided by the invention, the europium oxide and the neodymium oxide can be modified by the lamellar graphene, the size, the morphology and the content of the nano europium oxide and neodymium oxide particles codoped on the surface of the graphene can be regulated and controlled by controlling the content ratio of reactants and reaction conditions, and the Nd3+/Eu3+ ions are modified by the graphene, so that the purpose of enhancing the optical performance of the rare earth ions is realized.
4) The liquid material plasma spraying graphene modified temperature indicating thermal barrier coating provided by the invention effectively maintains the component content and uniform distribution of graphene in the coating. Avoids the loss caused by blowing away of high-speed and high-temperature spraying flame flow in the spraying process of preparing the graphene temperature indicating thermal barrier coating by adopting the traditional thermal spraying technology,
5) according to the temperature-indicating thermal barrier coating prepared by adopting the liquid material plasma thermal spraying technology, on one hand, the strength and toughness of the coating can be improved by the graphene, and in addition, the graphene/Nd 3+/Eu3+ is dispersedly distributed in the coating to serve as a second phase toughening coating, so that the effect of inhibiting cracks of the coating and relaxing stress is achieved, and the thermal barrier coating has great significance for improving the high-temperature service performance of the thermal barrier coating.
Drawings
Fig. 1 is a structural schematic diagram of a graphene modified temperature-indicating thermal barrier coating.
FIG. 2 is a scanning electron microscope image of graphene-modified europium oxide and neodymium oxide co-doped yttrium oxide stabilized zirconia spray powder.
FIG. 3 is a scanning electron microscope image of a cross section of a thermal barrier coating with temperature indication prepared by liquid material plasma spraying.
Fig. 4 is a schematic diagram of the existence of "embedded" graphene inside the graphene modified temperature indicating thermal barrier coating.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments.
Example 1:
the invention provides a preparation method of a graphene modified temperature indicating thermal barrier coating, which comprises the following steps of 1: 2400g of zirconium oxide octahydrate (ZrOCl) was weighed2·8H2O) was dissolved in 5000ml of deionized water and mixed with stirring.
Step 2: 80g of yttrium oxide (Y) are weighed out2O3) 2g of europium oxide (Eu)2O3) And 1g of neodymium oxide (Nd)2O3) Dissolving the solid powder in 1000ml of 1mol/L diluted hydrochloric acid, and uniformly stirring at 500rpm/min for 30min for mixing.
And step 3: 2g of graphene oxide is weighed and dispersed in 500ml of absolute ethyl alcohol for ultrasonic oscillation to prepare the graphene oxide dispersion liquid. The ultrasonic dispersion time is 120min, and the ultrasonic frequency is 15 Hz.
And 4, step 4: and (3) mixing the two solutions obtained in the step (2) and the step (3), keeping the temperature at 350 ℃ under a vacuum condition, and uniformly stirring for 30min by using a high-speed stirrer at the speed of 500 rpm/min.
And 5: mixing the mixed solution of zirconium oxide octahydrate obtained in the step (1) and the graphene modified Nd obtained in the step (4)3+/Eu3+The solution was stirred and mixed for a period of time while adding a suitable amount of polyethylene glycol (PEG 2000) dispersant. Keeping the temperature at 80 ℃, stirring for 60min at the stirring speed of 500rmp/min, and adding 30g of polyethylene glycol dispersant until the solution is in a uniform suspension state.
Step 6: preparation of PH =10 ammonia water (NH)3·H2O) reaction base liquid, gradually dripping ammonia water reaction base liquid into the solution obtained in the step 5, simultaneously heating the solution to keep the constant temperature of 80 ℃, and stirring for a certain time to obtain graphene modified Nd with the pH = 3-63+/Eu3+The yttria-stabilized zirconia (YSZ) precursor sol of (a).
And 7: by using hydrogen peroxide (H)2O2) Oxidizing agent oxidation and semipermeable membrane dialysis-Removing, and titrating with silver nitrate until no white AgCl flocculent precipitate is generated to obtain Cl-free solution-Modified Nd of graphene3+/Eu3+The yttria-stabilized zirconia sol of (a).
And 8: a matrix sample used for preparing the coating is 45 steel, and the matrix is degreased by acetone, and then is subjected to conventional ultrasonic cleaning and surface sand blasting pretreatment so as to improve the roughness and the activation degree of the matrix surface. And spraying a NiCoCrAIY bonding bottom layer with the thickness less than or equal to 0.1mm on the pretreated substrate by using a traditional powder plasma spraying process, and then spraying a graphene modified temperature-indicating thermal barrier coating by using liquid-phase plasma. The parameters of the liquid material plasma spraying process comprise 28L/min of argon (Ar) flow, 8L/min of hydrogen (H2) flow, 70V of spraying voltage, 550A of spraying current, 80mm of spraying distance and graphene modified Nd3+/Eu3+The sol rate of the Yttria Stabilized Zirconia (YSZ) precursor is 100g/min, the preheating temperature of the matrix is 500 ℃, and the pressure of the precursor liquid material conveying gas is 0.4 MPa.
As shown in FIG. 1, the structural diagram of the graphene modified temperature indicating thermal barrier coating prepared by the example is shown, the thickness of a first surface layer close to a NiCoCrAIY bonding bottom layer is about 50-60 μm, wherein the mass percentage of the graphene is 2%, the thickness of each surface layer is about 50-60 μm, and the content of the graphene is 1.5%, 1% and 0.5% respectively.
FIG. 2 is a scanning electron microscope image of the sprayed powder after drying and ball milling treatment of the graphene-modified europium oxide and neodymium oxide co-doped yttrium oxide stabilized zirconia sol prepared in the example. It can be seen that the prepared powder has uniform particle size, and graphene is dispersed and blended in the powder.
Fig. 3 shows the structure morphology of the cross section of the graphene modified temperature-indicating thermal barrier coating prepared by the example, and it can be seen that the coating structure is uniform and compact, the coating and the matrix are well combined, and no inclusion, pores or microcracks exist in the combined interface.
Fig. 4 is a high-power scanning electron microscope image of the graphene embedded inside the graphene modified temperature-indicating thermal barrier coating, and as shown by an arrow in the figure, it can be seen that the transparent graphene oxide of the nano thin layer is embedded inside the coating tissue, which indicates that the liquid plasma spraying effectively retains the existence of the graphene in the coating.
Example 2:
on the basis of the foregoing embodiment, this embodiment provides a preparation method of a graphene modified temperature indicating thermal barrier coating, including step 1: 4800g of zirconium oxide octahydrate (ZrOCl) was weighed2·8H2O) was dissolved in 10000ml of deionized water and mixed with stirring.
Step 2: 160g of yttrium oxide (Y) are weighed out2O3) 4g of europium oxide (Eu)2O3) And 2g of neodymium oxide (Nd)2O3) The solid powder was dissolved in 2000ml of 1mol/L diluted hydrochloric acid and mixed by stirring at 500rpm/min for 50 min.
And step 3: weighing 4g of graphene oxide, dispersing in 1000ml of absolute ethyl alcohol, and performing ultrasonic oscillation to prepare a graphene oxide dispersion liquid. The ultrasonic dispersion time is 150min, and the ultrasonic frequency is 15 Hz.
And 4, step 4: and (3) mixing the two solutions obtained in the step (2) and the step (3), keeping the temperature at 360 ℃ under a vacuum condition, and uniformly stirring for 60min by using a high-speed stirrer at the speed of 500 rpm/min.
And 5: mixing the mixed solution of zirconium oxide octahydrate obtained in the step (1) and the graphene modified Nd obtained in the step (4)3+/Eu3+The solution was stirred and mixed for a period of time while adding a suitable amount of polyethylene glycol (PEG 2000) dispersant. Keeping the temperature at 80 deg.C, stirring for 90min at 500rmp/min, and adding 50g polyethylene glycol dispersant until the solution is in uniform suspension state.
Step 6: preparation of aqueous Ammonia (NH) pH =103·H2O) reaction base solution, gradually dripping ammonia water reaction base solution into the solution obtained in the step 5, and simultaneously dripping ammonia water reaction base solution into the solutionHeating the solution to keep the constant temperature of 80 ℃, and stirring for a certain time to obtain the graphene modified Nd with the pH = 3-63+/Eu3+The yttria-stabilized zirconia (YSZ) precursor sol of (a).
And 7: by using hydrogen peroxide (H)2O2) Oxidizing agent oxidation and semipermeable membrane dialysis-Removing, and titrating with silver nitrate until no white AgCl flocculent precipitate is generated to obtain Cl-free solution-Modified Nd of graphene3+/Eu3+The yttria-stabilized zirconia sol of (a).
And 8: a matrix sample used for preparing the coating is 45 steel, and the matrix is degreased by acetone, and then is subjected to conventional ultrasonic cleaning and surface sand blasting pretreatment so as to improve the roughness and the activation degree of the matrix surface. And spraying a NiCoCrAIY bonding bottom layer with the thickness less than or equal to 0.1mm on the pretreated substrate by using a traditional powder plasma spraying process, and then spraying a graphene modified temperature-indicating thermal barrier coating by using liquid-phase plasma. The parameters of the liquid material plasma spraying process are that the flow of argon (Ar) is 32L/min, the flow of hydrogen (H2) is 10L/min, the spraying voltage is 70V, the spraying current is 570A, the spraying distance is 100mm, and the graphene modified Nd is3+/Eu3+The sol rate of the Yttria Stabilized Zirconia (YSZ) precursor is 120g/min, the preheating temperature of the matrix is 500 ℃, and the pressure of the precursor liquid material conveying gas is 0.4 MPa. The thickness of the NiCoCrAIY bonding bottom layer is about 20 microns, the thickness of the first surface layer close to the NiCoCrAIY bonding bottom layer is about 50-60 microns, the mass percentage of graphene is 2%, the thickness of each surface layer is about 50-60 microns, and the content of graphene is 1.5%, 1% and 0.5% respectively.
Example 3:
on the basis of the foregoing embodiment, this embodiment provides a preparation method of a graphene modified temperature indicating thermal barrier coating, including step 1: 1200g of zirconium oxide octahydrate (ZrOCl) was weighed2·8H2O) was dissolved in 2500ml of deionized water and mixed with stirring.
Step 2: weighing 40g of yttrium oxide (Y)2O3) 1g of europium oxide (Eu)2O3) And 0.5g of neodymium oxide (Nd)2O3) Solid powder dissolved in 500ml of 1mol/L dilute hydrochloric acidThe mixture was stirred at 500rpm/min for 30min and mixed.
And step 3: 2g of graphene oxide is weighed and dispersed in 500ml of absolute ethyl alcohol for ultrasonic oscillation to prepare the graphene oxide dispersion liquid. The ultrasonic dispersion time is 120min, and the ultrasonic frequency is 15 Hz.
And 4, step 4: and (3) mixing the two solutions obtained in the step (2) and the step (3), keeping the temperature at 350 ℃ under a vacuum condition, and uniformly stirring for 30min by using a high-speed stirrer at the speed of 500 rpm/min.
And 5: mixing the mixed solution of zirconium oxide octahydrate obtained in the step (1) and the graphene modified Nd obtained in the step (4)3+/Eu3+The solution was stirred and mixed for a period of time while adding a suitable amount of polyethylene glycol (PEG 2000) dispersant. Keeping the temperature at 80 ℃, stirring for 60min at the stirring speed of 500rmp/min, and adding 30g of polyethylene glycol dispersant until the solution is in a uniform suspension state.
Step 6: preparation of aqueous Ammonia (NH) pH =103·H2O) reaction base liquid, gradually dripping ammonia water reaction base liquid into the solution obtained in the step 5, simultaneously heating the solution to keep the constant temperature of 80 ℃, and stirring for a certain time to obtain graphene modified Nd with the pH = 3-63+/Eu3+The yttria-stabilized zirconia (YSZ) precursor sol of (a).
And 7: by using hydrogen peroxide (H)2O2) Oxidizing agent oxidation and semipermeable membrane dialysis-Removing, and titrating with silver nitrate until no white AgCl flocculent precipitate is generated to obtain Cl-free solution-Modified Nd of graphene3+/Eu3+The yttria-stabilized zirconia sol of (a).
And 8: a matrix sample used for preparing the coating is 45 steel, and the matrix is degreased by acetone, and then is subjected to conventional ultrasonic cleaning and surface sand blasting pretreatment so as to improve the roughness and the activation degree of the matrix surface. And spraying a NiCoCrAIY bonding bottom layer with the thickness less than or equal to 0.1mm on the pretreated substrate by using a traditional powder plasma spraying process, and then spraying a graphene modified temperature-indicating thermal barrier coating by using liquid-phase plasma. The parameters of the liquid material plasma spraying process are argon (Ar) flow 36L/min and hydrogen (H)2) The flow rate is 13L/min, the spraying voltage is 75V, and spraying is carried outCurrent 620A, spraying distance 110mm, graphene modified Nd3+/Eu3+The sol rate of the Yttria Stabilized Zirconia (YSZ) precursor is 140g/min, the preheating temperature of the matrix is 600 ℃, and the pressure of the precursor liquid material conveying gas is 0.5 MPa. The thickness of the NiCoCrAIY bonding bottom layer is about 20 microns, the thickness of the first surface layer close to the NiCoCrAIY bonding bottom layer is about 50-60 microns, the mass percentage of graphene is 2%, the thickness of each surface layer is about 50-60 microns, and the content of graphene is 1.5%, 1% and 0.5% respectively.
Example 4:
on the basis of the foregoing embodiment, this embodiment provides a preparation method of a graphene modified temperature indicating thermal barrier coating, including step 1: 4200g of zirconium oxide octahydrate (ZrOCl) was weighed2·8H2O) was dissolved in 10000ml of deionized water and mixed with stirring.
Step 2: weighing 140g of yttrium oxide (Y)2O3) 4g of europium oxide (Eu)2O3) And 2g of neodymium oxide (Nd)2O3) The solid powder was dissolved in 2000ml of 1mol/L diluted hydrochloric acid and mixed by stirring at 500rpm/min for 50 min.
And step 3: weighing 4g of graphene oxide, dispersing in 500ml of absolute ethyl alcohol, and performing ultrasonic oscillation to prepare a graphene oxide dispersion liquid. The ultrasonic dispersion time is 140min, and the ultrasonic frequency is 15 Hz.
And 4, step 4: and (3) mixing the two solutions obtained in the step (2) and the step (3), keeping the temperature at 350 ℃ under a vacuum condition, and uniformly stirring for 50min by using a high-speed stirrer at the speed of 500 rpm/min.
And 5: mixing the mixed solution of zirconium oxide octahydrate obtained in the step (1) and the graphene modified Nd obtained in the step (4)3+/Eu3+The solution was stirred and mixed for a period of time while adding a suitable amount of polyethylene glycol (PEG 2000) dispersant. Keeping the temperature at 80 deg.C, stirring for 60min at 500rmp/min, and adding 50g polyethylene glycol dispersant until the solution is in uniform suspension state.
Step 6: preparation of aqueous Ammonia (NH) pH =103·H2O) reaction base solution, gradually dripping ammonia water reaction base solution into the solution obtained in the step 5, and simultaneously addingKeeping the constant temperature of the hot solution at 80 ℃, and stirring for a certain time to obtain the graphene modified Nd with the pH = 3-63+/Eu3+The yttria-stabilized zirconia (YSZ) precursor sol of (a).
And 7: by using hydrogen peroxide (H)2O2) Oxidizing agent oxidation and semipermeable membrane dialysis-Removing, and titrating with silver nitrate until no white AgCl flocculent precipitate is generated to obtain Cl-free solution-Modified Nd of graphene3+/Eu3+The yttria-stabilized zirconia sol of (a).
And 8: a matrix sample used for preparing the coating is 45 steel, and the matrix is degreased by acetone, and then is subjected to conventional ultrasonic cleaning and surface sand blasting pretreatment so as to improve the roughness and the activation degree of the matrix surface. And spraying a NiCoCrAIY bonding bottom layer with the thickness less than or equal to 0.1mm on the pretreated substrate by using a traditional powder plasma spraying process, and then spraying a graphene modified temperature-indicating thermal barrier coating by using liquid-phase plasma. The parameters of the liquid material plasma spraying process are argon (Ar) flow of 40L/min and hydrogen (H)2) The flow is 15L/min, the spraying voltage is 80V, the spraying current is 660A, the spraying distance is 120mm, and the graphene modified Nd3+/Eu3+The sol rate of the Yttria Stabilized Zirconia (YSZ) precursor is 150g/min, the preheating temperature of the matrix is 700 ℃, and the conveying gas pressure of the precursor liquid material is 0.6 MPa. The thickness of the NiCoCrAIY bonding bottom layer is about 20 microns, the thickness of the first surface layer close to the NiCoCrAIY bonding bottom layer is about 50-60 microns, the mass percentage of graphene is 2%, the thickness of each surface layer is about 50-60 microns, and the content of graphene is 1.5%, 1% and 0.5% respectively.
Compared with the closest prior art, the invention has the following beneficial effects:
1) compared with the difficulty that the service temperature of a YSZ thermal barrier coating prepared by traditional thermal spraying cannot be known, the liquid material graphene modified europium oxide and neodymium oxide co-doped yttrium oxide stabilized zirconia precursor sol and the temperature indicating thermal barrier coating prepared by adopting the liquid material plasma spraying technology can monitor the temperature change in the full thickness range inside the thermal barrier coating in real time, can play a role in early warning the failure of the coating and can monitor the integrity and the safe service condition of the thermal barrier coating.
2) Compared with the single rare earth ion Eu3+ applied to the high temperature of the thermal barrier coating, the difficulty of weak fluorescence intensity exists, and the high-sensitivity response of the fluorescence intensity ratio can be realized in a wider temperature range for preparing the temperature-indicating thermal barrier coating through a synergistic action mechanism of Nd3+/Eu3+ co-doping.
3) According to the technical scheme provided by the invention, the europium oxide and the neodymium oxide can be modified by the lamellar graphene, the size, the morphology and the content of the nano europium oxide and neodymium oxide particles codoped on the surface of the graphene can be regulated and controlled by controlling the content ratio of reactants and reaction conditions, and the Nd3+/Eu3+ ions are modified by the graphene, so that the purpose of enhancing the optical performance of the rare earth ions is realized.
4) The liquid material plasma spraying graphene modified temperature indicating thermal barrier coating provided by the invention effectively maintains the component content and uniform distribution of graphene in the coating. Avoids the loss caused by blowing away of high-speed and high-temperature spraying flame flow in the spraying process of preparing the graphene temperature indicating thermal barrier coating by adopting the traditional thermal spraying technology,
5) according to the temperature-indicating thermal barrier coating prepared by adopting the liquid material plasma thermal spraying technology, on one hand, the strength and toughness of the coating can be improved by the graphene, and in addition, the graphene/Nd 3+/Eu3+ is dispersedly distributed in the coating to serve as a second phase toughening coating, so that the effect of inhibiting cracks of the coating and relaxing stress is achieved, and the thermal barrier coating has great significance for improving the high-temperature service performance of the thermal barrier coating.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (1)
1. A preparation method of a graphene oxide modified temperature-indicating thermal barrier coating is characterized by comprising the following steps:
step 1: weighing a certain amount of zirconium oxychloride octahydrate (ZrOCl)2·8H2O) dissolving in deionized water, and stirring and mixing;
step 2:weighing a certain amount of yttrium oxide (Y)2O3) Europium oxide (Eu)2O3) And neodymium oxide (Nd)2O3) Dissolving solid powder in 1mol/L dilute hydrochloric acid, and stirring and mixing;
and step 3: weighing a certain amount of graphene oxide, dispersing the graphene oxide in absolute ethyl alcohol, and performing ultrasonic oscillation to prepare a graphene oxide dispersion liquid;
and 4, step 4: mixing the two solutions obtained in the step 2 and the step 3, and stirring for a certain time at a certain rotating speed within a certain temperature range under a vacuum condition until the solution is in a uniform suspension state;
and 5: mixing the mixed solution of zirconium oxychloride octahydrate obtained in the step (1) and the Nd modified by the graphene oxide obtained in the step (4)3+/Eu3+Stirring and mixing the solution for a certain time, and simultaneously adding a proper amount of polyethylene glycol dispersant;
step 6: preparation of aqueous ammonia (NH) at pH 103·H2O) reaction base liquid, gradually dropping ammonia water reaction base liquid into the solution obtained in the step 5, simultaneously heating the solution to keep the constant temperature of 80 ℃, and stirring for a certain time to obtain the graphene oxide modified Nd with the pH value of 3-63+/Eu3+The yttria-stabilized zirconia (YSZ) precursor sol of (a);
and 7: by using hydrogen peroxide (H)2O2) Oxidizing agent oxidation and semipermeable membrane dialysis－Removing, and titrating with silver nitrate until no white AgCl flocculent precipitate is generated to obtain Cl-free solution－Nd modified by graphene oxide3+/Eu3+The yttria-stabilized zirconia sol of (a);
and 8: the matrix sample used for preparing the coating is 45 steel, the matrix is deoiled by acetone at first, then conventional ultrasonic cleaning and surface sand blasting pretreatment are carried out to improve the roughness and the activation degree of the matrix surface, NiCoCrAIY bonding bottom layer with the thickness less than or equal to 0.1mm is sprayed on the pretreated matrix by using the traditional powder plasma spraying process, and then liquid phase plasma is adopted to spray oxidized graphene modified temperature indicating thermal barrier coating; zirconium oxychloride octahydrate (ZrOCl) in steps 1 and 22·8H2O) and yttrium oxide (Y)2O3) The mass ratio is 28-30: 1; europium oxide (Eu) in the step 22O3) And neodymium oxide (Nd)2O3) Mixing with dilute hydrochloric acid; wherein the mass ratio of europium oxide to neodymium oxide is 1.5-2: 1, uniformly stirring for 30-60 min at the speed of 500rpm by a high-speed stirrer; and 3, dispersing a certain amount of graphene oxide in absolute ethyl alcohol, and performing ultrasonic oscillation to prepare a graphene oxide dispersion liquid, wherein the mass ratio of the graphene oxide to the absolute ethyl alcohol is 1: 100-300 ℃, keeping the temperature at 80-100 ℃, and performing ultrasonic dispersion for 120-180 min at an ultrasonic frequency of 15 Hz; in the step 4, the two solutions obtained in the step 2 and the step 3 are mixed, the temperature is kept at 350-400 ℃ under the vacuum condition, and a high-speed stirrer is used for uniformly stirring for 30-60 min at the speed of 500 rpm; stirring the mixed solution in the step 5 for 60-90 min at the stirring speed of 500rpm, and adding 30-50 g of polyethylene glycol dispersant; the liquid material plasma spraying process parameters of the graphene oxide modified temperature indicating thermal barrier coating prepared in the step 8 are argon (Ar) flow rate of 28-40L/min and hydrogen (H)2) The flow rate is 8-15L/min, the spraying voltage is 70-80V, the spraying current is 550-660A, the spraying distance is 80-120 mm, and the graphene oxide is used for modifying Nd3+/Eu3+The sol rate of the yttria-stabilized zirconia (YSZ) precursor is 100-150 g/min, the preheating temperature of the matrix is 500-700 ℃, and the pressure of the precursor liquid material conveying gas is 0.3-0.6 MPa; the graphene oxide modified temperature indicating thermal barrier coating prepared in the step 8 is a gradient composite coating, the bottom layer is a NiCoCrAIY bonding bottom layer, the graphene oxide modified temperature indicating thermal barrier coating is a surface layer, the surface layer is divided into 4 layers, the thickness of each layer is 50-60 mu m, the total thickness is 200-240 mu m, the thickness is close to the NiCoCrAIY bonding bottom layer to the surface of the surface layer, and the graphene oxide modified temperature indicating thermal barrier coating contains 2% of graphene oxide, 1.5% of graphene oxide, 1% of graphene oxide and 0.5% of graphene oxide in percentage by mass.
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