CN107400846A - A kind of graphene is modified the preparation method of temperature indicating thermal barrier coating - Google Patents
A kind of graphene is modified the preparation method of temperature indicating thermal barrier coating Download PDFInfo
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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
- C23C4/12—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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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7784—Chalcogenides
- C09K11/7787—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
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
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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
- C23C4/04—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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- 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
- C23C4/04—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
Abstract
The present invention provides the preparation method that a kind of graphene is modified temperature indicating thermal barrier coating, comprises the following steps：Step 1：Eight water zirconium oxides are dissolved in deionized water；Step 2：Yittrium oxide, europium oxide and neodymia solid powder are dissolved in watery hydrochloric acid；Step 3：Graphene oxide is dispersed in absolute ethyl alcohol；Step 4：Two kinds of solution obtained by step 2 and step 3 are mixed；Step 5：Step 1 mixed liquor and step 4 resulting solution are stirred and add polyethylene glycol dispersant；Step 6：The ammoniacal liquor reaction bottom liquid of PH=10 is prepared, while heated solution obtains yttria-stabilized zirconia precursor sol；Step 7：Obtain the yttria-stabilized zirconia colloidal sol that the graphene without Cl is modified Nd3+/Eu3+；Step 8：Temperature indicating thermal barrier coating is modified using liquid phase plasma spraying graphene.The problem of scaling loss, slip by, reunite during plasma spray technology prepares coating present invention, avoiding nanoscale graphene be present.
Description
Technical field
The invention belongs to the preparation of graphene modified RE fluorescent particles combined oxidation yttrium stable zirconium oxide precursor solution
Technique, graphene are modified the design of temperature indicating thermal barrier coating and the technology field of plasma spraying with liquid feedstock prepares coating, especially
Refer to the preparation method that a kind of graphene is modified temperature indicating thermal barrier coating.
Background technology
At present, wide variety of thermal barrier coating system is obtained in aero-engine by alloy substrate, MCrAlY or Pt to be changed
Property aluminide tack coat, thermally grown oxide (TGO) and the part group of yttria-stabilized zirconia (YSZ) ceramic with heat resistance layer four
Into.Thermal barrier coating life prediction is largely dependent upon the temperature survey of application environment.First, thermal barrier coating process under arms
Middle surface temperature Ts is more much higher than substrate surface temperatures Tb, it has been reported that the temperature of metal bonding coating is increased to from 1010 DEG C
1064 DEG C, only 54 DEG C of difference TGO can just grown with 3 times of speed, cause the premature failure of thermal barrier coating.But at present
Thermometric mode can not all be competent at this work：On the one hand because measuring point is in the lower section of thermal barrier coating ceramic topcoats, tradition
Thermometric mode can not touch；On the other hand because gas turbine internal temperature is high, strong electromagnetic, narrow space, leaf be present
Piece such as runs at high speed at a series of unfavorable thermometric conditions.Therefore, the new thermal barrier coating with real time temperature response characteristic is developed,
The inherent law between coating service temperature and service life is studied, to effectively assessing coating military service health status, realizes thermal boundary
The early warning failure of coating is significant.
The thermometry used in high temperature environments at present mainly has infrared measurement of temperature and thermocouple temperature measurement [6], wherein infrared
Thermometry belongs to contactless temperature-measuring, has temperature-measuring range wide, is not limited by the thermometric upper limit, will not also destroy measurand
Temperature field, the advantages that reaction rate is fast.But it is limited in that the emissivity for being vulnerable to object, measurement distance, flue dust and water
The influence of the extraneous factors such as vapour, measurement error is larger, in high temperature environments by being influenceed to be particularly acute.Thermocouple is a kind of profit
With the contacting temperature measurement method of pyroelectric effect, although this method has simple to operate, reliability and the high advantage of measurement accuracy,
Because temperature element must carry out sufficient heat exchange with measured medium, thermometric mesh could be realized by reaching thermal balance within a certain period of time
, so the delay phenomenon of thermometric be present, while limited by exotic material, it is impossible to measured applied to very high temperature.
In recent years, the fluorescence thermometry based on material optic response temperature characterisitic develops rapidly, for monitoring thermal boundary in real time
Coating service temperature and predict that its service life brings hope.Its principle is by the rare earth doped fluorescence inside thermal barrier coating
Element, when thermal barrier coating by different temperatures environment military service after, the spectral width of fluorescent material, fluorescence intensity, fluorescence lifetime meeting
Corresponding change occurs therewith, thus thermal barrier coating service temperature can be supervised in real time by studying the relevance realization of itself and temperature
The purpose of survey.
In recent years, the thermometric research that rare-earth fluorescent element is applied to thermal barrier coating starts to be paid close attention to by researcher.
Gentleman M M [9] are carried out to the mapping relations being on active service in the range of the fluorescence intensity of Eu3+ doping YSZ coatings and 0 ~ 1200 DEG C
Research, and the decline curve of the temperature range undercoating fluorescence intensity is given, provide for scientific forecasting coating residual life
Theoretical foundation.Chen X et al. have studied YSZ powder doping Dy3+ and plasma spraying YSZ:The fluorescence intensity of Dy3+ coatings
Change, and establish fluorescence decay cycle and the mapping relations of coating military service at 0 ~ 1000 DEG C.Pin L et al. have studied colloidal sol and coagulate
Rare earth doped film prepared by glue sedimentation, and confirm the application of Tm3+ elements at relatively high temperatures.Eldridge J I
Trial adds a small amount of rare earth in YSZ, by means of the characteristic wavelength of fluorescence and the temperature change of biometrics coat inside, so that
The condition of high temperature of coating can be monitored in real time.
At home, using the health status research in rare-earth fluorescent intensity evaluation thermal barrier coating high-temperature service also in starting
Stage.Maritime Affairs University Of Dalian Zhou Feng et al. is prepared for adulterating Eu3+ and Dy3+ SrAl2O4 coatings using plasma spraying, to it
Luminescent properties are characterized, the Primary Study luminous mechanisms of Eu3+ and Dy3+ in the coating.
In summary, weak in coat inside radiation intensity for rare-earth luminescent material, hot environment is strong after being on active service for a long time
Spend the problem to decay rapidly.This item purpose Research Thinking is to carry out codope and modification to existing rare earth element first, to reality
The purpose of existing " multiplication " its radiation intensity.Eu3+ is more as thermal barrier coating fluorescence doped chemical research at this stage, has been found
There is preferable photoresponse temperature characterisitic in hot environment.In addition, the Rare Earth Functional Materials enhancing fluorescence spoke of double activator doping
Intensity is penetrated to be paid close attention in recent years, there are some researches show, the energy transmission to Eu3+ be present in Nd3+, and with the rise of temperature
Rate of energy transfer becomes big, and the wide scope response that fluorescence intensity varies with temperature can be achieved if codope is carried out.Separately
Outside, graphene oxide（GO）It is the derivative of graphene, substantial amounts of oxygen-containing functional group is contained on its surface, and graphene has fluorescence special
Property principle be exactly in graphene oxidizing process caused oxygen-containing functional group cause π tracks occur defect and cause.Also there is research
Prove that GO surface oxygen functional groups can influence the change of fluorescence intensity and position.To sum up analyze, using graphene be modified Tb3+/
Eu3+ composition regulation and control and preparation can be achieved the single Eu3+ of enhancing and be applied to the problem that fluorescence intensity is weak in thermal barrier coating.
Therefore, the prior art is defective, it is necessary to improve.
The content of the invention
The present invention proposes that a kind of graphene is modified temperature indicating thermal barrier coating and preparation method, plasma spray technology can be used to prepare
Temperature indicating thermal barrier coating with photoresponse temperature characterisitic, on-line identification can be changed by the spectral energy of rare-earth fluorescent element and gone out
Coating integrity situation.It is expected to realize that temperature of the coating in Life cycle monitors in real time, reaches to coating failure early warning
Purpose, to establish accurate Life Prediction Model based theoretical.
The technical problems to be solved by the invention are in view of the shortcomings of the prior art, there is provided a kind of graphene is modified temperature indicating heat
The preparation method of barrier coating.
Technical scheme is as follows：
A kind of graphene is modified the preparation method of temperature indicating thermal barrier coating, comprises the following steps：
Step 1：Weigh a certain amount of eight water zirconium oxide（ZrOCl2·8H2O）It is dissolved in deionized water, is stirred mixing；
Step 2：Weigh a certain amount of yittrium oxide（Y2O3）, europium oxide（Eu2O3）And neodymia（Nd2O3）Solid powder, it is dissolved in 1
In mol/L watery hydrochloric acid, mixing is stirred；
Step 3：Weigh a certain amount of graphene oxide and be dispersed in ultrasonic vibration preparation graphene oxide dispersion in absolute ethyl alcohol；
Step 4：Two kinds of solution of gained in step 2 and step 3 are mixed, under vacuum condition, necessarily to turn in certain temperature range
Speed stirring certain time, until solution is in even suspension state；
Step 5：Eight water zirconium oxide mixed liquors obtained by step 1 and step 4 gained graphene are modified Nd3+/Eu3+Solution is stirred
Mixing certain time is mixed, while adds appropriate polyethylene glycol（PEG2000）Dispersant；
Step 6：Prepare the ammoniacal liquor (NH of PH=103·H2O bottom liquid) is reacted, gradually ammoniacal liquor is reacted in the liquid of bottom and dripped to obtained by step 5
Solution, while heated solution keeps 80 DEG C of constant temperature, stirs certain time, the graphene for obtaining PH=3 ~ 6 is modified Nd3+/Eu3+Oxygen
Change yttrium stable zirconium oxide（YSZ）Precursor sol；
Step 7：Utilize hydrogen peroxide（H2O2）Oxidizing and half membrane dialyzing is by Cl-Remove, while observed with silver nitrate titration
Untill not having white AgCl flocculent deposits generation, acquisition is free of Cl-Graphene be modified Nd3+/Eu3+Yttria-stabilized zirconia
Colloidal sol；
Step 8：The matrix used sample of prepares coating is 45 steel, and matrix is deoiled with acetone first, conventional Ultrasound is carried out again and cleans
And surface sand-blasting pretreatment, to improve the roughness of matrix surface and activation grade.Traditional powder is used on the matrix of pretreatment
After last plasma spray coating process spraying≤0.1mm NiCoCrAIY bond coatings, it is modified using liquid phase plasma spraying graphene
Temperature indicating thermal barrier coating.
In above-mentioned, eight water zirconium oxide in the step 1 and 2（ZrOCl2·8H2O）With yittrium oxide（Y2O3）Mass percent
For 28 ~ 30:1.
In above-mentioned, europium oxide in the step 2（Eu2O3）And neodymia（Nd2O3）Mixed using watery hydrochloric acid；Wherein aoxidize
Europium is 1.5 ~ 2 with neodymia mass percent:1, homogenizer with 500rpm/min speed, the processing 30min that stirs ~
60min。
In above-mentioned, a certain amount of graphene oxide is dispersed in ultrasonic vibration in absolute ethyl alcohol and prepares oxidation stone in the step 3
Black alkene dispersion liquid, wherein graphene oxide are 1 with absolute ethyl alcohol mass percent:100 ~ 300, temperature is kept for 80 ~ 100 DEG C, is surpassed
Sound jitter time is 120min ~ 180min, supersonic frequency 15Hz.
In above-mentioned, two kinds of solution obtained by step 2 and step 3 are mixed in the step 4, under vacuum condition, temperature is kept
350 ~ 400 DEG C, homogenizer is with 500rpm/min speed, and stir processing 30min ~ 60min.
In above-mentioned, the step 5 mixed solution mixing time is 60 ~ 90min, speed of agitator 500rmp/min, is added
30g ~ 50g polyethylene glycol dispersants.
In above-mentioned, the plasma spraying with liquid feedstock technological parameter that the step 8 prepares graphene modification temperature indicating thermal barrier coating is
Argon gas（Ar）28 ~ 40L/min of flow, hydrogen（H2）8 ~ 15L/min of flow, 70 ~ 80V of spray voltage, 550 ~ 660A of spraying current,
80 ~ 120mm of spray distance, graphene are modified Nd3+/Eu3+Yttria-stabilized zirconia（YSZ）Precursor sol speed 100 ~
150g/min, 500 ~ 700 DEG C of substrate preheating temperature, 0.3 ~ 0.6MPa of presoma liquid material conveying gas pressure.
In above-mentioned, graphene modification temperature indicating thermal barrier coating prepared by the step 8 is gradient composite coating, and bottom is
NiCoCrAIY bond coatings, it is surface layer that graphene, which is modified temperature indicating thermal barrier coating, and surface layer is divided into 4 layers, per a layer thickness about 50 ~
60 μm, about 300 ~ 350 μm of gross thickness, close to NiCoCrAIY bond coatings to facing surface, each layer graphene is modified temperature indicating heat
Barrier coating inside is respectively 2%, 1.5%, 1% and 0.5% containing graphene weight/mass percentage composition.
Compared with immediate prior art, the invention has the advantages that：
1）The YSZ thermal barrier coatings prepared compared to traditional thermal spraying can not learn the problem of its service temperature, liquid provided by the invention
Expect europium oxide and neodymia codope yttria-stabilized zirconia precursor sol that graphene is modified, and using liquid material etc. from
Sub- spraying technology, which prepares temperature indicating thermal barrier coating, can monitor temperature change inside thermal barrier coating in the range of through thickness in real time, can be with
Forewarning function is played to coating failure, monitors thermal barrier coating integrality and safe duty status.
2）Compared to single rare earth ion Eu3+ in thermal barrier coating high temperature application, the weak problem of fluorescence intensity be present, the present invention
By the synergy mechanism of Nd3+/Eu3+ codopes, can be prepared in realization real in temperature indicating thermal barrier coating wide temperature range
The highly sensitive response of existing fluorescence intensity ratio.
3）Technical scheme provided by the invention can be reacted in the modified oxidized europium of Sheet Graphite alkene and neodymia by controlling
Content ratio between thing, and reaction condition, it is possible to achieve the chi of graphenic surface co-doped nano europium oxide and neodymia particle
Very little, pattern, content regulation and control, are modified using graphene to Nd3+/Eu3+ ions, realize enhancing rare earth ion optical property
Purpose.
4）It is provided by the invention that stone has been effectively kept using plasma spraying with liquid feedstock graphene modification temperature indicating thermal barrier coating
The component content of black alkene in the coating and it is uniformly distributed.Avoid and the painting of graphene temperature indicating thermal boundary is prepared using traditional plasma spray technology
Layer blows winged and lost in spraying process by the spraying flame stream of high speed, high temperature,
5）Provided by the invention to prepare temperature indicating thermal barrier coating using liquid material plasma thermal sprayed technology, on the one hand graphene can carry
The intensity and toughness of high coating, furthermore with graphene/Nd3+/Eu3+ Dispersed precipitates in coat inside as secondary phase toughening
Coating, while play a part of that coating occurs in crackle with suppression and stress relaxation, the high-temperature service to improving thermal barrier coating
Performance makes great sense.
Brief description of the drawings
Fig. 1 is that graphene is modified temperature indicating thermal insulation layer construction schematic diagram.
Fig. 2 is the europium oxide and neodymia codope yttria-stabilized zirconia dusty spray ESEM that graphene is modified
Figure.
Fig. 3 is that plasma spraying with liquid feedstock prepares temperature indicating thermal barrier coating cross-sectional scans electron microscope.
Fig. 4 is that " embedded " that graphene is modified graphene inside temperature indicating thermal barrier coating has schematic diagram.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1：
The present invention provides the preparation method that a kind of graphene is modified temperature indicating thermal barrier coating, including step 1：Weigh the water oxygens of 2400g eight
Change zirconium（ZrOCl2·8H2O）It is dissolved in 5000ml deionized waters, is stirred mixing.
Step 2：Weigh 80g yittrium oxide（Y2O3）, 2g europium oxides（Eu2O3）With 1g neodymia（Nd2O3）Solid powder, it is dissolved in
1000ml concentration is in 1 mol/L watery hydrochloric acid, and with 500rpm/min speed, the processing 30min that stirs is mixed.
Step 3：Weigh 2g graphene oxides and be dispersed in ultrasonic vibration in 500ml absolute ethyl alcohols and prepare graphene oxide and disperse
Liquid.The ultrasonic disperse time is 120min, supersonic frequency 15Hz.
Step 4：Two kinds of solution obtained by step 2, step 3 are mixed, under vacuum condition, temperature is kept for 350 DEG C, high-speed stirred
Machine is with 500rpm/min speed, and stir processing 30min.
Step 5：Eight water zirconium oxide mixed liquors obtained by step 1 and step 4 gained graphene are modified Nd3+/Eu3+Solution enters
Row is stirred certain time, while adds appropriate polyethylene glycol（PEG2000）Dispersant.Keeping temperature is 80 DEG C, during stirring
Between be 60min, speed of agitator 500rmp/min, 30g polyethylene glycol dispersants are added, until solution is in even suspension state.
Step 6：Prepare the ammoniacal liquor (NH of PH=103·H2O bottom liquid) is reacted, gradually ammoniacal liquor is reacted in the liquid of bottom and drips to step 5
Resulting solution, while heated solution keeps 80 DEG C of constant temperature, stirs certain time, the graphene for obtaining PH=3 ~ 6 is modified Nd3+/Eu3+
Yttria-stabilized zirconia（YSZ）Precursor sol.
Step 7：Utilize hydrogen peroxide（H2O2）Oxidizing and half membrane dialyzing is by Cl-Remove, while use silver nitrate titration
Untill observing no white AgCl flocculent deposits generation, acquisition is free of Cl-Graphene be modified Nd3+/Eu3+Stabilized with yttrium oxide oxygen
Change zirconium colloidal sol.
Step 8：The matrix used sample of prepares coating is 45 steel, and matrix is deoiled with acetone first, carries out conventional Ultrasound again
Cleaning and surface sand-blasting pretreatment, to improve the roughness of matrix surface and activation grade.Tradition is used on the matrix of pretreatment
Powder plasma spraying coating process spraying≤0.1mm NiCoCrAIY bond coatings after, using liquid phase plasma spraying graphene
Modified temperature indicating thermal barrier coating.Plasma spraying with liquid feedstock technological parameter is argon gas（Ar）Flow 28L/min, hydrogen（H2）Flow 8L/
Min, spray voltage 70V, spraying current 550A, spray distance 80mm, graphene are modified Nd3+/Eu3+Stabilized with yttrium oxide oxidation
Zirconium（YSZ）Precursor sol speed 100g/min, 500 DEG C of substrate preheating temperature, presoma liquid material conveying gas pressure 0.4MPa.
Graphene is prepared for the example as shown in Figure 1 and be modified temperature indicating thermal insulation layer construction schematic diagram, glued close to NiCoCrAIY
About 50 ~ 60 μm of the first layer surface thickness of bottom is tied, wherein graphene weight/mass percentage composition is 2%, to totally four layers, every layer of surface layer
About 50 ~ 60 μm of thickness, graphene content is respectively 1.5%, 1% and 0.5%.
Fig. 2 is the europium oxide and neodymia codope yttria-stabilized zirconia colloidal sol that graphene prepared by the example is modified
Dusty spray low power scanning electron microscope (SEM) photograph after drying ball-milling treatment.As can be seen that the powder particle epigranular prepared, inside powder
Disperse blending has graphene.
Fig. 3 is that graphene prepared by the example is modified temperature indicating thermal barrier coating section structure pattern, it can be seen that coating structure
Even compact, coating are combined preferably with matrix, combination interface without be mingled with, hole and micro-crack exist.
Fig. 4 is that graphene is modified inside temperature indicating thermal barrier coating high power scanning electron microscope (SEM) photograph existing for graphene " embedded ", such as
It can be seen that the transparence graphene oxide of nano thin-layer is embedded in inside coating structure shown in arrow in figure, illustrate liquid material etc. from
Son spraying effectively remains the presence of graphene in the coating.
Embodiment 2：
On the basis of above-described embodiment, the present embodiment provides the preparation method that a kind of graphene is modified temperature indicating thermal barrier coating, bag
Include step 1：Weigh the water zirconium oxides of 4800g eight（ZrOCl2·8H2O）It is dissolved in 10000ml deionized waters, is stirred mixing.
Step 2：Weigh 160g yittrium oxide（Y2O3）, 4g europium oxides（Eu2O3）With 2g neodymia（Nd2O3）Solid powder, it is molten
In the watery hydrochloric acid that 2000ml concentration is 1 mol/L, with 500rpm/min speed, the processing 50min that stirs is mixed.
Step 3：Weigh 4g graphene oxides and be dispersed in ultrasonic vibration in 1000ml absolute ethyl alcohols and prepare graphene oxide point
Dispersion liquid.The ultrasonic disperse time is 150min, supersonic frequency 15Hz.
Step 4：Two kinds of solution obtained by step 2, step 3 are mixed, under vacuum condition, temperature is kept for 360 DEG C, high-speed stirred
Machine is with 500rpm/min speed, and stir processing 60min.
Step 5：Eight water zirconium oxide mixed liquors obtained by step 1 and step 4 gained graphene are modified Nd3+/Eu3+Solution enters
Row is stirred certain time, while adds appropriate polyethylene glycol（PEG2000）Dispersant.Keeping temperature is 80 DEG C, during stirring
Between be 90min, speed of agitator 500rmp/min, 50g polyethylene glycol dispersants are added, until solution is in even suspension state.
Step 6：Prepare the ammoniacal liquor (NH of PH=103·H2O bottom liquid) is reacted, gradually ammoniacal liquor is reacted in the liquid of bottom and drips to step 5
Resulting solution, while heated solution keeps 80 DEG C of constant temperature, stirs certain time, the graphene for obtaining PH=3 ~ 6 is modified Nd3+/Eu3+
Yttria-stabilized zirconia（YSZ）Precursor sol.
Step 7：Utilize hydrogen peroxide（H2O2）Oxidizing and half membrane dialyzing is by Cl-Remove, while use silver nitrate titration
Untill observing no white AgCl flocculent deposits generation, acquisition is free of Cl-Graphene be modified Nd3+/Eu3+Stabilized with yttrium oxide oxygen
Change zirconium colloidal sol.
Step 8：The matrix used sample of prepares coating is 45 steel, and matrix is deoiled with acetone first, carries out conventional Ultrasound again
Cleaning and surface sand-blasting pretreatment, to improve the roughness of matrix surface and activation grade.Tradition is used on the matrix of pretreatment
Powder plasma spraying coating process spraying≤0.1mm NiCoCrAIY bond coatings after, using liquid phase plasma spraying graphene
Modified temperature indicating thermal barrier coating.Plasma spraying with liquid feedstock technological parameter is argon gas（Ar）Flow 32L/min, hydrogen（H2）Flow 10L/
Min, spray voltage 70V, spraying current 570A, spray distance 100mm, graphene are modified Nd3+/Eu3+Stabilized with yttrium oxide oxidation
Zirconium（YSZ）Precursor sol speed 120g/min, 500 DEG C of substrate preheating temperature, presoma liquid material conveying gas pressure 0.4MPa.
About 20 μm of NiCoCrAIY bond coatings thickness is prepared, close to the μ of first layer surface thickness about 50 ~ 60 of NiCoCrAIY bond coatings
M, wherein graphene weight/mass percentage composition are 2%, and to totally four layers of surface layer, per about 50 ~ 60 μm of thickness degree, graphene content is respectively
1.5%th, 1% and 0.5%.
Embodiment 3：
On the basis of above-described embodiment, the present embodiment provides the preparation method that a kind of graphene is modified temperature indicating thermal barrier coating, bag
Include step 1：Weigh the water zirconium oxides of 1200g eight（ZrOCl2·8H2O）It is dissolved in 2500ml deionized waters, is stirred mixing.
Step 2：Weigh 40g yittrium oxide（Y2O3）, 1g europium oxides（Eu2O3）With 0.5g neodymia（Nd2O3）Solid powder, it is molten
In the watery hydrochloric acid that 500ml concentration is 1 mol/L, with 500rpm/min speed, the processing 30min that stirs is mixed.
Step 3：Weigh 2g graphene oxides and be dispersed in ultrasonic vibration in 500ml absolute ethyl alcohols and prepare graphene oxide and disperse
Liquid.The ultrasonic disperse time is 120min, supersonic frequency 15Hz.
Step 4：Two kinds of solution obtained by step 2, step 3 are mixed, under vacuum condition, temperature is kept for 350 DEG C, high-speed stirred
Machine is with 500rpm/min speed, and stir processing 30min.
Step 5：Eight water zirconium oxide mixed liquors obtained by step 1 and step 4 gained graphene are modified Nd3+/Eu3+Solution enters
Row is stirred certain time, while adds appropriate polyethylene glycol（PEG2000）Dispersant.Keeping temperature is 80 DEG C, during stirring
Between be 60min, speed of agitator 500rmp/min, 30g polyethylene glycol dispersants are added, until solution is in even suspension state.
Step 6：Prepare the ammoniacal liquor (NH of PH=103·H2O bottom liquid) is reacted, gradually ammoniacal liquor is reacted in the liquid of bottom and drips to step 5
Resulting solution, while heated solution keeps 80 DEG C of constant temperature, stirs certain time, the graphene for obtaining PH=3 ~ 6 is modified Nd3+/Eu3+
Yttria-stabilized zirconia（YSZ）Precursor sol.
Step 7：Utilize hydrogen peroxide（H2O2）Oxidizing and half membrane dialyzing is by Cl-Remove, while use silver nitrate titration
Untill observing no white AgCl flocculent deposits generation, acquisition is free of Cl-Graphene be modified Nd3+/Eu3+Stabilized with yttrium oxide oxygen
Change zirconium colloidal sol.
Step 8：The matrix used sample of prepares coating is 45 steel, and matrix is deoiled with acetone first, carries out conventional Ultrasound again
Cleaning and surface sand-blasting pretreatment, to improve the roughness of matrix surface and activation grade.Tradition is used on the matrix of pretreatment
Powder plasma spraying coating process spraying≤0.1mm NiCoCrAIY bond coatings after, using liquid phase plasma spraying graphene
Modified temperature indicating thermal barrier coating.Plasma spraying with liquid feedstock technological parameter is argon gas（Ar）Flow 36L/min, hydrogen（H2）Flow 13L/
Min, spray voltage 75V, spraying current 620A, spray distance 110mm, graphene are modified Nd3+/Eu3+Stabilized with yttrium oxide oxidation
Zirconium（YSZ）Precursor sol speed 140g/min, 600 DEG C of substrate preheating temperature, presoma liquid material conveying gas pressure 0.5MPa.
About 20 μm of NiCoCrAIY bond coatings thickness is prepared, close to the μ of first layer surface thickness about 50 ~ 60 of NiCoCrAIY bond coatings
M, wherein graphene weight/mass percentage composition are 2%, and to totally four layers of surface layer, per about 50 ~ 60 μm of thickness degree, graphene content is respectively
1.5%th, 1% and 0.5%.
Example 4：
On the basis of above-described embodiment, the present embodiment provides the preparation method that a kind of graphene is modified temperature indicating thermal barrier coating, bag
Include step 1：Weigh the water zirconium oxides of 4200g eight（ZrOCl2·8H2O）It is dissolved in 10000ml deionized waters, is stirred mixing.
Step 2：Weigh 140g yittrium oxide（Y2O3）, 4g europium oxides（Eu2O3）With 2g neodymia（Nd2O3）Solid powder, it is molten
In the watery hydrochloric acid that 2000ml concentration is 1 mol/L, with 500rpm/min speed, the processing 50min that stirs is mixed.
Step 3：Weigh 4g graphene oxides and be dispersed in ultrasonic vibration in 500ml absolute ethyl alcohols and prepare graphene oxide and disperse
Liquid.The ultrasonic disperse time is 140min, supersonic frequency 15Hz.
Step 4：Two kinds of solution obtained by step 2, step 3 are mixed, under vacuum condition, temperature is kept for 350 DEG C, high-speed stirred
Machine is with 500rpm/min speed, and stir processing 50min.
Step 5：Eight water zirconium oxide mixed liquors obtained by step 1 and step 4 gained graphene are modified Nd3+/Eu3+Solution enters
Row is stirred certain time, while adds appropriate polyethylene glycol（PEG2000）Dispersant.Keeping temperature is 80 DEG C, during stirring
Between be 60min, speed of agitator 500rmp/min, 50g polyethylene glycol dispersants are added, until solution is in even suspension state.
Step 6：Prepare the ammoniacal liquor (NH of PH=103·H2O bottom liquid) is reacted, gradually ammoniacal liquor is reacted in the liquid of bottom and drips to step 5
Resulting solution, while heated solution keeps 80 DEG C of constant temperature, stirs certain time, the graphene for obtaining PH=3 ~ 6 is modified Nd3+/Eu3+
Yttria-stabilized zirconia（YSZ）Precursor sol.
Step 7：Utilize hydrogen peroxide（H2O2）Oxidizing and half membrane dialyzing is by Cl-Remove, while use silver nitrate titration
Untill observing no white AgCl flocculent deposits generation, acquisition is free of Cl-Graphene be modified Nd3+/Eu3+Stabilized with yttrium oxide oxygen
Change zirconium colloidal sol.
Step 8：The matrix used sample of prepares coating is 45 steel, and matrix is deoiled with acetone first, carries out conventional Ultrasound again
Cleaning and surface sand-blasting pretreatment, to improve the roughness of matrix surface and activation grade.Tradition is used on the matrix of pretreatment
Powder plasma spraying coating process spraying≤0.1mm NiCoCrAIY bond coatings after, using liquid phase plasma spraying graphene
Modified temperature indicating thermal barrier coating.Plasma spraying with liquid feedstock technological parameter is argon gas（Ar）Flow 40L/min, hydrogen（H2）Flow 15L/
Min, spray voltage 80V, spraying current 660A, spray distance 120mm, graphene are modified Nd3+/Eu3+Stabilized with yttrium oxide oxidation
Zirconium（YSZ）Precursor sol speed 150g/min, 700 DEG C of substrate preheating temperature, presoma liquid material conveying gas pressure 0.6MPa.
About 20 μm of NiCoCrAIY bond coatings thickness is prepared, close to the μ of first layer surface thickness about 50 ~ 60 of NiCoCrAIY bond coatings
M, wherein graphene weight/mass percentage composition are 2%, and to totally four layers of surface layer, per about 50 ~ 60 μm of thickness degree, graphene content is respectively
1.5%th, 1% and 0.5%.
Compared with immediate prior art, the invention has the advantages that：
1）The YSZ thermal barrier coatings prepared compared to traditional thermal spraying can not learn the problem of its service temperature, liquid provided by the invention
Expect europium oxide and neodymia codope yttria-stabilized zirconia precursor sol that graphene is modified, and using liquid material etc. from
Sub- spraying technology, which prepares temperature indicating thermal barrier coating, can monitor temperature change inside thermal barrier coating in the range of through thickness in real time, can be with
Forewarning function is played to coating failure, monitors thermal barrier coating integrality and safe duty status.
2）Compared to single rare earth ion Eu3+ in thermal barrier coating high temperature application, the weak problem of fluorescence intensity be present, the present invention
By the synergy mechanism of Nd3+/Eu3+ codopes, can be prepared in realization real in temperature indicating thermal barrier coating wide temperature range
The highly sensitive response of existing fluorescence intensity ratio.
3）Technical scheme provided by the invention can be reacted in the modified oxidized europium of Sheet Graphite alkene and neodymia by controlling
Content ratio between thing, and reaction condition, it is possible to achieve the chi of graphenic surface co-doped nano europium oxide and neodymia particle
Very little, pattern, content regulation and control, are modified using graphene to Nd3+/Eu3+ ions, realize enhancing rare earth ion optical property
Purpose.
4）It is provided by the invention that stone has been effectively kept using plasma spraying with liquid feedstock graphene modification temperature indicating thermal barrier coating
The component content of black alkene in the coating and it is uniformly distributed.Avoid and the painting of graphene temperature indicating thermal boundary is prepared using traditional plasma spray technology
Layer blows winged and lost in spraying process by the spraying flame stream of high speed, high temperature,
5）Provided by the invention to prepare temperature indicating thermal barrier coating using liquid material plasma thermal sprayed technology, on the one hand graphene can carry
The intensity and toughness of high coating, furthermore with graphene/Nd3+/Eu3+ Dispersed precipitates in coat inside as secondary phase toughening
Coating, while play a part of that coating occurs in crackle with suppression and stress relaxation, the high-temperature service to improving thermal barrier coating
Performance makes great sense.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted, and institute
There is the protection domain that these modifications and variations should all belong to appended claims of the present invention.
Claims (8)
1. a kind of graphene is modified the preparation method of temperature indicating thermal barrier coating, it is characterised in that comprises the following steps：
Step 1：Weigh a certain amount of eight water zirconium oxide（ZrOCl2·8H2O）It is dissolved in deionized water, is stirred mixing；
Step 2：Weigh a certain amount of yittrium oxide（Y2O3）, europium oxide（Eu2O3）And neodymia（Nd2O3）Solid powder, it is dissolved in 1
In mol/L watery hydrochloric acid, mixing is stirred；
Step 3：Weigh a certain amount of graphene oxide and be dispersed in ultrasonic vibration preparation graphene oxide dispersion in absolute ethyl alcohol；
Step 4：Two kinds of solution of gained in step 2 and step 3 are mixed, under vacuum condition, necessarily to turn in certain temperature range
Speed stirring certain time, until solution is in even suspension state；
Step 5：Eight water zirconium oxide mixed liquors obtained by step 1 and step 4 gained graphene are modified Nd3+/Eu3+Solution is stirred
Certain time is mixed, while adds appropriate polyethylene glycol（PEG2000）Dispersant；
Step 6：Prepare the ammoniacal liquor (NH of PH=103·H2O bottom liquid) is reacted, gradually ammoniacal liquor is reacted in the liquid of bottom and dripped to obtained by step 5
Solution, while heated solution keeps 80 DEG C of constant temperature, stirs certain time, the graphene for obtaining PH=3 ~ 6 is modified Nd3+/Eu3+Oxygen
Change yttrium stable zirconium oxide（YSZ）Precursor sol；
Step 7：Utilize hydrogen peroxide（H2O2）Oxidizing and half membrane dialyzing is by Cl-Remove, while observed with silver nitrate titration
Untill not having white AgCl flocculent deposits generation, acquisition is free of Cl-Graphene be modified Nd3+/Eu3+Yttria-stabilized zirconia
Colloidal sol；
Step 8：The matrix used sample of prepares coating is 45 steel, and matrix is deoiled with acetone first, conventional Ultrasound is carried out again and cleans
And surface sand-blasting pretreatment, to improve the roughness of matrix surface and activation grade.Traditional powder is used on the matrix of pretreatment
After last plasma spray coating process spraying≤0.1mm NiCoCrAIY bond coatings, it is modified using liquid phase plasma spraying graphene
Temperature indicating thermal barrier coating.
2. according to claim 1 and preparation method, it is characterised in that eight water zirconium oxide in the step 1 and 2
（ZrOCl2·8H2O）With yittrium oxide（Y2O3）Mass percent is 28 ~ 30:1.
3. preparation method according to claim 1, it is characterised in that europium oxide in the step 2（Eu2O3）And neodymia
（Nd2O3）Mixed using watery hydrochloric acid；Wherein europium oxide and neodymia mass percent are 1.5 ~ 2:1, homogenizer with
500rpm/min speed, stir processing 30min ~ 60min.
4. preparation method according to claim 1, it is characterised in that a certain amount of graphene oxide disperses in the step 3
Ultrasonic vibration prepares graphene oxide dispersion in absolute ethyl alcohol, and wherein graphene oxide is with absolute ethyl alcohol mass percent
1:100 ~ 300, temperature is kept for 80 ~ 100 DEG C, and the ultrasonic disperse time is 120min ~ 180min, supersonic frequency 15Hz.
5. preparation method according to claim 1, it is characterised in that by two obtained by step 2 and step 3 in the step 4
Kind solution is mixed, and under vacuum condition, temperature is kept for 350 ~ 400 DEG C, and homogenizer is with 500rpm/min speed, and stir place
Manage 30min ~ 60min.
6. preparation method according to claim 1, it is characterised in that the step 5 mixed solution mixing time be 60 ~
90min, speed of agitator 500rmp/min, add 30g ~ 50g polyethylene glycol dispersants.
7. preparation method according to claim 1, it is characterised in that the step 8 prepares graphene and is modified temperature indicating thermal boundary
The plasma spraying with liquid feedstock technological parameter of coating is argon gas（Ar）28 ~ 40L/min of flow, hydrogen（H2）8 ~ 15L/min of flow, spray
70 ~ 80V of voltage, 550 ~ 660A of spraying current, 80 ~ 120mm of spray distance are applied, graphene is modified Nd3+/Eu3+Stabilized with yttrium oxide
Zirconium oxide（YSZ）Precursor sol 100 ~ 150g/min of speed, 500 ~ 700 DEG C of substrate preheating temperature, presoma liquid material conveying gas
0.3 ~ 0.6MPa of body pressure.
8. preparation method according to claim 1, it is characterised in that graphene prepared by the step 8 is modified temperature indicating thermal boundary
Coating is gradient composite coating, and bottom is NiCoCrAIY bond coatings, and it is surface layer that graphene, which is modified temperature indicating thermal barrier coating, surface layer
4 layers are divided into, per about 50 ~ 60 μm of a layer thickness, about 300 ~ 350 μm of gross thickness, close to NiCoCrAIY bond coatings to surface layer table
Face, it is respectively 2%, 1.5%, 1% and that each layer graphene, which is modified inside temperature indicating thermal barrier coating containing graphene weight/mass percentage composition,
0.5%。
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