CN109468639B - Ultra-limit zirconium alloy and preparation method thereof - Google Patents

Ultra-limit zirconium alloy and preparation method thereof Download PDF

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CN109468639B
CN109468639B CN201811640624.4A CN201811640624A CN109468639B CN 109468639 B CN109468639 B CN 109468639B CN 201811640624 A CN201811640624 A CN 201811640624A CN 109468639 B CN109468639 B CN 109468639B
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zirconium alloy
ceramic
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limit
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CN109468639A (en
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冯晶
李超
宋鹏
种晓宇
葛振华
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Shaanxi Tianxuan Coating Technology Co ltd
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Kunming University of Science and Technology
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Priority to JP2021538453A priority patent/JP7242867B2/en
Priority to EP19903063.6A priority patent/EP3904555A4/en
Priority to US17/419,250 priority patent/US11530485B2/en
Priority to PCT/CN2019/117283 priority patent/WO2020134655A1/en
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    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
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Abstract

The invention belongs to the technical field of zirconium alloy metal materials, and discloses a super-limit zirconium alloy and a preparation method thereof. The ultra-limit zirconium alloy comprises a zirconium alloy matrix, wherein a bonding layer, a noble metal layer, a ceramic A layer, a ceramic B layer, a sealing coating, a reflecting layer, a catadioptric layer and an electric insulating layer are sequentially deposited on the surface of the zirconium alloy matrix. The preparation method of the ultra-limit zirconium alloy comprises the step of sequentially depositing a bonding layer, a noble metal layer, a ceramic A layer, a ceramic B layer, a sealing coating, a reflecting layer, a catadioptric layer and an electric insulating layer on the surface of a zirconium alloy substrate to form the ultra-limit zirconium alloy. The use temperature of the super-limit zirconium alloy provided by the invention is increased to be higher than the melting point of the original zirconium alloy by 100-500 ℃, and the super-limit zirconium alloy can be used at the super-limit temperature.

Description

Ultra-limit zirconium alloy and preparation method thereof
Technical Field
The invention belongs to the field of zirconium alloy metal materials, and particularly relates to a super-limit zirconium alloy and a preparation method thereof.
Background
The zirconium alloy is an alloy which takes zirconium as a matrix and is added with other elements. Zirconium alloys have very low thermal neutron absorption cross-sections, high hardness, ductility, and corrosion resistance, and are commonly used in the nuclear technology field, for example, in the fabrication of fuel rods in nuclear reactors. Due to the limitation of the use environment, the zirconium alloy must have good high-temperature oxidation resistance and corrosion resistance, be not easy to fall off and lose efficacy during the use process, be convenient for long-term maintenance, have high stability performance in extreme environments (such as exceeding the limit temperature (exceeding the melting point)), and the like. The melting point of the zirconium alloy is about 1850 ℃, and the use temperature is only about 70% of the melting point, so that the use of the existing zirconium alloy in the nuclear technology is still limited to a certain extent, so that the fuel rod made of the zirconium alloy has short service life and cannot stably run for a long time.
Disclosure of Invention
The invention aims to provide a super-limit zirconium alloy and a preparation method thereof, and aims to solve the problem that the conventional zirconium alloy cannot stably operate in a nuclear reaction technology for a long time.
In order to achieve the purpose, the invention provides the following technical scheme that the ultra-limit zirconium alloy comprises a zirconium alloy substrate, wherein a bonding layer, a noble metal layer, a ceramic A layer and a ceramic B layer are sequentially deposited on the surface of the zirconium alloy substrate.
The beneficial effects of the technical scheme are as follows:
the inventors have made extensive studies on zirconium alloys in an attempt to improve the zirconium alloys so as to satisfy the long-term stable operation of the zirconium alloys in the use of nuclear technology. In the process of continuous trial of the inventor, the inventor discovers that the use temperature of the zirconium alloy can be increased by 100-500 ℃ by depositing a coating with a certain proportion on the surface of the zirconium alloy, and the use temperature of the material can be increased by a few degrees centigrade in a high-temperature environment, so that the method is very difficult to achieve, and a great breakthrough is obtained in the use of the zirconium alloy, so that the zirconium alloy can stably operate for a long time in the use of the nuclear technology.
According to the technical scheme, the bonding layer, the precious metal layer, the ceramic A layer and the ceramic B layer are deposited on the zirconium alloy substrate, so that the service temperature of the zirconium alloy can be greatly increased, and the zirconium alloy is suitable for being used at the ultra-limit temperature. The bonding layer is deposited, so that the bonding effect between each coating and the zirconium alloy matrix can be improved, and the coating is prevented from falling off in the using process; the deposited noble metal layer can avoid oxygen diffusion into the coating, thereby avoiding the oxidation of the zirconium alloy matrix. The ceramic A layer and the ceramic B layer are deposited, so that the heat conduction can be reduced, and the service temperature of the zirconium alloy matrix can be increased.
In summary, the present invention has the following technical effects:
1. the ultra-limit zirconium alloy provided by the invention can overcome the problem that the original zirconium alloy is in service for a long time in a high-temperature and high-pressure steam environment so that the surface of the zirconium alloy is oxidized and falls off; when the high-temperature high.
2. According to the invention, the multilayer coating is deposited on the surface of the zirconium alloy substrate, so that the use temperature of the zirconium alloy substrate can be raised to be higher than the melting point of the original zirconium alloy substrate by 100-.
3. The super-limit zirconium alloy provided by the invention has excellent corrosion resistance, so that the service time under acidic or alkaline conditions is greatly increased, the waste caused by material corrosion can be reduced, and the cost is saved.
4. The ultra-limit zirconium alloy provided by the invention breaks through the development bottleneck of the traditional zirconium alloy, the service temperature of the zirconium alloy can be further improved on the basis of higher melting point, and the improved temperature is a dramatic progress. The ultra-limit zirconium alloy provided by the invention can be stably used for a long time at an ultra-limit temperature.
Furthermore, the thickness of the bonding layer is 50-150 microns, the thickness of the noble metal layer is 10-20 microns, the thickness of the ceramic layer A is 50-80 microns, the thickness of the ceramic layer B is 50-80 microns, and a sealing coating layer with the thickness of 5-10 microns, a reflecting layer with the thickness of 10-15 microns, a catadioptric layer with the thickness of 10-15 microns and an electric insulating layer with the thickness of 15-20 microns are sequentially deposited on the surface of the ceramic layer B.
Has the advantages that: the sealing coating can isolate external oxidation or corrosion atmosphere, so that the external atmosphere cannot directly react with the internal coating, and the service life of the coating is prolonged; the reflecting layer has the effect of reflecting a heat source, so that the heat source on the surface of the zirconium alloy is reduced, and the use temperature is increased. The deposited catadioptric layer can block the refraction of infrared rays in the coating, thereby reducing the temperature of the zirconium alloy matrix and improving the service temperature of the prepared zirconium alloy. The electric insulating layer can isolate conductive ions, and the corrosion of the conductive ions to the zirconium alloy matrix is avoided, so that the corrosion resistance of the prepared ultra-limit zirconium alloy is improved. According to the technical scheme, the coating layers and the thickness of the coating layers are matched, so that the service temperature of the zirconium alloy is greatly increased, and the aircraft is convenient to manufacture and use.
Further, the bonding layer comprises MCrAlY, wherein MCrAlY is CoCrAlY, NiCoCrAlY or CoNiCrAlY; the noble metal layer is one or more of Pt, Ru, Rh, Pd, Ir and Os alloy.
Has the advantages that: the proportion of elements in NiCoCrAlY and CoNiCrAlY is different, so that the prepared materials are different. The bonding layer has good bonding effect, so that the subsequent coating has good bonding effect with the zirconium alloy body, and the falling probability of the coating is reduced; the noble metal has the characteristic of oxidation resistance, and can effectively prevent oxygen from diffusing into the bonding layer and the zirconium alloy matrix at high temperature, so that the oxidation resistance of the coating is improved, and the service life of the coating is prolonged.
Further, the component of the ceramic A layer is Y2O3-ZrO2、Y2O3-CeO2、Y2O3-TiO2、Y2O3-Yb2O3、Y2O3-Er2O3、Y2O3-Dy2O3、Y2O3-HfO2One or a mixture of several of them; the ceramic B layer is RETaO4，RETaO4Is spherical and has a particle size of 10-70 μm.
Has the advantages that: YSZ or rare earth zirconate, a commonly used material as a thermal barrier coating, is readily available. The RETaO4 has the characteristics of low thermal conductivity and high expansion, the low thermal conductivity can reduce the conduction of heat, so that the zirconium alloy matrix keeps low temperature in a high-temperature environment, and the service temperature of the prepared zirconium alloy is increased; the high expansion coefficient is matched with the thermal expansion coefficient of the bonding layer, and the thermal expansion coefficient of the noble metal bonding layer is also larger, so that the thermal mismatch stress (stress generated by different thermal expansion coefficients) of the ceramic layer and the bonding layer is smaller in the thermal cycle process (namely the process of continuously heating and cooling), and the service life of the coating is further prolonged. (in a popular way, when two coatings with larger difference of thermal expansion coefficients are deposited together and the temperature is raised or lowered, the expansion degrees of the two coatings are seriously different, so that the stress between the two coatings is increased, and cracks or even falling-off is caused between the two coatings.)
Further, the component of the sealing coating is Ti3SiC，REPO4And BN, or a mixture of more than one of the BN and the BN.
Has the advantages that: the material can isolate external oxidation or corrosion atmosphere, so that the external atmosphere can not directly react with the coating inside, and the service life of the coating is prolonged.
Further, the reflective layer has a composition of REVO4、RETaO4、Y2O3One or a mixture of several of them; the component of the catadioptric layer is graphene, and the graphene is in a disordered arrangement state in spatial distribution.
Has the advantages that: REVO4、RETaO4、Y2O3The reflection coefficient of the zirconium alloy is high, so that a heat source can be reflected, the heat radiation is reduced, and the temperature of a zirconium alloy matrix is reduced, so that the service temperature of the prepared zirconium alloy is increased; although the graphene has a higher refractive index, when incident light irradiates on the catadioptric layer, the randomly arranged graphene can enhance the refraction of the light in all directions, so that the incident light is prevented from being refracted in the same direction, the refraction dispersion effect is achieved, and the incident light intensity entering the coating is reduced
Further, the electric insulation layer is made of one or a mixture of more of polytetrafluoroethylene, polyimide, polyphenyl ether, polyphenylene sulfide, polyether ether ketone, bismaleimide, furan resin, cyanate resin and polyarylethynyl.
Has the advantages that: the material can isolate conductive ions, and the situation that the conductive ions enter the zirconium alloy matrix to corrode the zirconium alloy matrix is avoided.
The invention also provides another technical scheme, and the preparation method of the ultra-limit zirconium alloy comprises the following steps:
the method comprises the following steps:
depositing a 50-150 mu m thick bonding layer on the surface of the zirconium alloy substrate;
step two:
depositing a layer of noble metal layer with the thickness of 10-20 mu m on the surface of the bonding layer;
step three:
depositing a ceramic A layer with the thickness of 50-80 mu m on the surface of the noble metal;
step four:
depositing a 50-80 mu m thick ceramic layer B on the surface of the ceramic layer A;
step five:
depositing a sealing coating layer with the thickness of 5-10 mu m on the surface of the ceramic B layer;
step six:
depositing a reflecting layer with the thickness of 10-15 microns on the surface of the sealing coating;
step seven:
depositing a 10-15 mu m-thick catadioptric layer on the surface of the reflecting layer;
step eight:
and depositing an electric insulating layer with the thickness of 15-20 mu m on the surface of the catadioptric layer so as to prepare the super-limit zirconium alloy.
The beneficial effects of the technical scheme are as follows:
by controlling the thickness of each coating deposited on the zirconium alloy substrate, the service temperature of the prepared ultra-limit zirconium alloy can be increased to 100-500 ℃ higher than the melting point of the original zirconium alloy, and the prepared ultra-limit zirconium alloy has excellent corrosion resistance. Meanwhile, the situation that the weight of the prepared ultra-limit zirconium alloy is increased greatly due to the fact that the thickness of the coating is large can be avoided, and therefore the ultra-limit zirconium alloy can meet the use requirements of airplanes.
Furthermore, the total thickness of the bonding layer, the noble metal layer, the ceramic layer A, the ceramic layer B, the sealing coating, the reflecting layer, the catadioptric layer and the electric insulating layer is 185-320 mu m.
Has the advantages that: the coating with the thickness can ensure that the prepared super-limit zirconium alloy has good heat resistance and corrosion resistance, and the weight of the super-limit zirconium alloy is not greatly increased, so that the prepared super-limit zirconium alloy can meet the use requirements of airplanes.
Further, in the first step, before the bonding layer is deposited, oil stains on the surface of the zirconium alloy substrate are removed; and performing sand blasting treatment on the surface of the zirconium alloy matrix to ensure that the surface roughness of the zirconium alloy matrix is 60-100 mu m.
Has the advantages that: the bonding effect between the zirconium alloy matrix and the coating can be improved by removing oil stains on the surface of the zirconium alloy matrix; the coating can generate larger internal stress in the curing process, and the problem of stress concentration can be effectively solved by utilizing the roughness of the surface of the zirconium alloy substrate subjected to sand blasting treatment by a sand blasting machine, so that the coating can be prevented from cracking. And the existence of the surface roughness can support the quality of a part of coating, which is beneficial to eliminating the sagging phenomenon.
Drawings
FIG. 1 is a schematic structural diagram of a super-limit zirconium alloy according to the present invention;
FIG. 2 is a graph showing the high temperature creep test of example 1 and comparative example 10 under 50MPa at 2000 deg.C;
FIG. 3 is a graph of salt spray corrosion experiments for example 1 and comparative example 10 of the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: zirconium alloy base member 1, tie coat 2, noble metal layer 3, pottery A layer 4, pottery B layer 5, seal coating 6, reflection stratum 7, catadioptric layer 8, electric insulating layer 9.
The invention provides a super-limit zirconium alloy, which comprises a zirconium alloy matrix 1, wherein a 50-150 mu m thick bonding layer 2, a 10-20 mu m thick noble metal layer 3, a 50-80 mu m thick ceramic A layer 4, a 50-80 mu m thick ceramic B layer 5, a 5-10 mu m thick sealing coating 6, a 10-15 mu m thick reflecting layer 7, a 10-15 mu m thick catadioptric layer 8 and a 15-20 mu m thick electric insulating layer 9 are sequentially deposited on the surface of the zirconium alloy matrix 1; wherein the zirconium alloy matrix 1 is added with zinc, aluminum, copper, tin, niobium, iron and chromiumAnd zirconium alloy of one or more elements of nickel. The bonding layer 2 comprises MCrAlY, wherein the MCrAlY is CoCrAlY, NiCoCrAlY or CoNiCrAlY; the component of the noble metal layer 3 is one or more of Pt, Ru, Rh, Pd, Ir and Os alloy; the component of the ceramic A layer 4 is Y2O3-ZrO2、Y2O3-CeO2、Y2O3-TiO2、Y2O3-CeO2、Y2O3-Yb2O3、Y2O3-Er2O3、Y2O3-Dy2O3、Y2O3-HfO2One or a mixture of several of them; the composition of the ceramic B layer 5 is RETaO4(RE＝Y、Nd、Eu、Gd、Dy、Er、Yb)，RETaO4Is spherical and has a particle size of 10-70 μm; the component of the sealing coating 6 is Ti3SiC，REPO4(RE ═ Nd, Eu, Gd, Dy, Er, Y, Yb) and one or a mixture of more of BN; the reflective layer 7 has a composition REVO4、RETaO4、Y2O3One or more of RE, Y, Nd, Eu, Gd, Dy, Er and Yb; the component of the catadioptric layer 8 is graphene, and the spatial distribution of the graphene is in a disordered arrangement state; the electric insulation layer 9 is made of one or a mixture of more of polytetrafluoroethylene, polyimide, polyphenyl ether, polyphenylene sulfide, polyether ether ketone, bismaleimide, furan resin, cyanate resin and polyarylethynyl.
The present invention utilizes RETaO4As the ceramic B layer, the ceramic B layer has the effects of low thermal conductivity and high expansion rate, and can reduce the heat conduction; and RETaO prepared by the following method4Can meet the requirements of APS spraying technology.
RETaO4The preparation method comprises the following steps:
step (1):
mixing rare earth oxide (RE)2O3) Powder, tantalum pentoxide (Ta)2O5) Pre-drying the powder at 600 ℃ for 8 h; weighing according to the molar ratio of 1:1Predried rare earth oxides (RE)2O3) Powder and tantalum pentoxide (Ta)2O5) Powder; adding the pre-dried powder into an ethanol solvent to obtain a mixed solution, wherein the molar ratio of RE to Ta in the mixed solution is 1: 1; and then ball milling is carried out on the mixed solution for 10 hours by adopting a ball mill, and the rotating speed of the ball mill is 300 r/min.
Drying the slurry obtained after ball milling by using a rotary evaporator (model: N-1200B), wherein the drying temperature is 60 ℃, the drying time is 2h, and sieving the dried powder by using a 300-mesh sieve to obtain powder A.
Step (2):
preparing the powder A obtained in the step (1) into RETaO by adopting a high-temperature solid-phase reaction method4The reaction temperature of the powder B is 1700 ℃, and the reaction time is 10 hours; and the powder B was sieved using a 300 mesh sieve.
And (3):
mixing the powder B sieved in the step (2) with a deionized water solvent and an organic adhesive to obtain slurry C, wherein the mass percent of the powder B in the slurry C is 25%, the mass percent of the organic adhesive is 2%, and the balance is the solvent, and the organic adhesive is polyvinyl alcohol or gum arabic; drying the slurry C by using a centrifugal atomization method at the temperature of 600 ℃ at the centrifugal speed of 8500r/min to obtain dried granules D;
and (4):
sintering the material particles D obtained in the step (3) at 1200 ℃ for 8h, and sieving the sintered material particles D by using a 300-mesh sieve to obtain spherical RETaO with the particle size of 10-70 nm4Ceramic powder.
The inventor finds out through a large number of experiments that the service temperature of the prepared ultra-limit zirconium alloy is high and the corrosion resistance is good within the parameter range provided by the invention, and 20 groups of the obtained ultra-limit zirconium alloy are listed for explanation in the invention.
The parameters of examples 1 to 20 of the super-limit zirconium alloy and the preparation method thereof of the present invention are shown in tables 1 and 2:
TABLE 1
Figure GDA0002293991000000061
Figure GDA0002293991000000071
Figure GDA0002293991000000081
Figure GDA0002293991000000091
TABLE 2
Figure GDA0002293991000000092
Figure GDA0002293991000000101
Figure GDA0002293991000000111
Figure GDA0002293991000000121
Now, a method for preparing a super-limit zirconium alloy according to another embodiment of the present invention will be described with reference to example 1.
A preparation method of a super-limit zirconium alloy comprises the following steps:
the method comprises the following steps:
in this embodiment, Zr-1Nb zirconium alloy is selected as zirconium alloy matrix, and oil stain and impurities on the surface of zirconium alloy matrix are removed by soaking method, firstly, zirconium alloy matrix is soaked in alkaline solution or emulsified cleaning solution, wherein the main components of emulsified cleaning solution are ethanol and surfactant, the main components of alkaline solution are sodium hydroxide, trisodium phosphate and sodium carbonate sodium silicate, and alkaline solution is used in this embodiment. Adjusting the pH value of the alkali solution to 10-11, soaking the zirconium alloy substrate in the alkali solution for 0.5-1.5h, taking out the zirconium alloy substrate, wherein the soaking time is 1h in the embodiment, and then washing the zirconium alloy substrate with clear water and drying the zirconium alloy substrate. Performing sand blasting treatment on the surface of the zirconium alloy substrate by using a sand blasting machine, wherein the used sand blasting machine is a JCK-SS500-6A automatic transmission type sand blasting machine, and the sand blasting material adopted in sand blasting is 23-mesh quartz sand; the surface roughness of the zirconium alloy matrix after sand blasting is 60-100 μm, and the surface roughness of the zirconium alloy matrix in the embodiment is 80 μm, so that the coating and the zirconium alloy matrix can be conveniently bonded.
Step two:
depositing a bonding layer on the surface of the Zr-1Nb zirconium alloy subjected to sand blasting, firstly spraying a layer of CoCrAlY with the thickness of 75 microns on the surface of a zirconium alloy matrix by using an HVOF method as the bonding layer, wherein the technological parameters of the HVOF method during spraying are that the pressure of oxygen is 0.4MPa and the flow rate is 250L/min respectively; c2H4The pressure and the flow rate of the pressure and the flow rate are respectively 0.4MPa and 55L/min; the length of the spray gun nozzle is 100mm, and the spraying distance is 100 mm.
Step three:
and depositing a layer of Pt with the thickness of 10um on the CoCrAlY by using an HVOF method to serve as a noble metal layer, wherein the technological parameters of the HVOF method during spraying are the same as those in the first step.
Step four:
spraying a layer of Y with the thickness of 50um on the surface of the noble metal layer by utilizing a plasma spraying technology2O3-Yb2O3When the ceramic layer A is used as a ceramic layer A, the technological parameters of the plasma spraying technology during spraying are that the flow of argon is 40L/min; the flow rate of hydrogen is 5L/min, the power is 30kW, the powder feeding amount is 20g/min, and the spraying distance is 100 mm.
Step five:
spraying a layer of YTaO with the thickness of 50 mu m on the ceramic A by utilizing a plasma spraying technology4And as the ceramic B layer, the spraying process parameters are the same as those in the fourth step.
Step six:
spraying a layer of Ti with the thickness of 5 mu m on the surface of the ceramic B layer by using an electron beam physical vapor deposition technology3SiC as sealing coating, electron beam physical gas phase in sprayingThe parameters of the deposition technology are that the argon pressure is 0.2Mpa, the power is 2kW, and the matrix temperature is 250 ℃.
Step seven:
spraying a layer of REVO with the thickness of 10um on the sealing coating by using an electron beam physical vapor deposition technology4And e, spraying the reflecting layer, wherein the spraying process parameters are the same as those in the sixth step.
Step eight:
uniformly mixing graphene and micron-sized carbon powder materials, introducing the mixed powder into a solution for ultrasonic vibration mixing, wherein the solution is an ethanol solution added with 1% of a dispersing agent, and separating the micron-sized carbon powder from the uniformly mixed solution by using filter paper. And coating the solution mixed with the graphene on the surface of the reflecting layer to serve as a catadioptric layer, putting the zirconium alloy coated with the graphene catadioptric layer into a drying oven, and drying at 60 ℃ for 2 hours, wherein the thickness of the coated catadioptric layer is 13 microns.
Step nine:
polyphenyl ether is adhered to the wool or the sponge, the sponge is used in the embodiment, the sponge adhered with the polyphenyl ether is tightly attached to the catadioptric layer, the polyphenyl ether is permeated to the surface of the catadioptric layer through high-speed vibration and friction of the sponge by a vibration polishing machine, and the thickness of the electric insulating layer is 15 microns.
Step ten:
the spray coating is provided with a bonding layer, a noble metal layer, a ceramic A layer, a ceramic B layer, a sealing coating, a reflecting layer, a catadioptric layer and an electric insulating layer zirconium alloy, and the aging treatment is carried out for 5-10 h at 50-80 ℃, the temperature used in the embodiment is 60 ℃ and the time is 8h, so that the internal stress of each coating is released, the bonding performance of the coating is improved, and finally the ultra-limit zirconium alloy is obtained.
Examples 2-20 differ from example 1 only in the parameters shown in table 1.
Experiment:
comparative experiments with the comparative examples 1-20 were carried out with set-up of 110 groups, and the parameters of comparative examples 1-9 are shown in Table 3:
TABLE 3
Figure GDA0002293991000000141
Figure GDA0002293991000000151
Figure GDA0002293991000000161
Comparative examples 1 to 9 differ from example 1 only in the respective parameters shown in table 3, and comparative example 10 is a Zr-1Nb zirconium alloy.
The following experiments were carried out using the zirconium alloys provided in examples 1 to 20 and comparative examples 1 to 10:
high temperature creep test:
the zirconium alloys provided in examples 1 to 20 and comparative examples 1 to 10 were processed into columnar test pieces 187mm in length and 16mm in diameter, and subjected to a high-temperature creep test using an electronic high-temperature creep rupture strength tester of type RMT-D5.
The test pieces of examples 1 to 20 and comparative examples 1 to 10 were placed in an electronic high-temperature creep rupture strength tester, and the tester was started to raise the temperature of the tester, and during the temperature raising, the test pieces were in an unstressed state (in the unstressed state, the test pieces were free to expand, and the high-temperature creep was deformed by the combined action of temperature and stress and increased with time, so that the rate of temperature rise did not affect the creep). When the temperature of the testing machine reached 2000 ℃, the testing machine was adjusted to a stress of 50MPa, and a high temperature creep test was conducted, taking example 1 and comparative example 10 as examples, the test results are shown in fig. 2 (a) shows comparative example 10, (B) shows example 1), and the specific test results of examples 1 to 20 and comparative examples 1 to 10 are shown in table 4.
As can be understood from FIG. 2, the (A) and (B) specimens have 3 stages of creep deformation, but at temperatures above the melting point of the ZR-1NB zirconium alloy, the (A) specimen undergoes creep rupture in a very short time, and it can be understood that the ZR-1NB zirconium alloy is hardly loaded at temperatures above the melting point of the ZR-1NB zirconium alloy. Compared with the test piece (A), the creep resistance of the test piece (B) is obviously improved, the steady-state creep time of the test piece (B) is longer, and the creep curve enters an accelerated creep stage and generates creep fracture after passing through a longer steady-state creep stage. Therefore, compared with the original ZR-1NB zirconium alloy, the super-limit zirconium alloy provided by the invention has the advantages that the super-limit zirconium alloy maintains better mechanical property without breaking and has excellent high temperature resistance at the temperature exceeding the melting point of the ZR-1NB zirconium alloy.
Salt spray corrosion test:
the zirconium alloys provided in examples 1 to 20 and comparative examples 1 to 10 were processed into 50mm × 25mm × 2mm test pieces, and then subjected to oil removal and rust removal treatment, cleaning, and drying. An YWX/Q-250B salt spray corrosion box is used as experimental equipment, and an atmospheric corrosion environment of GB/T2967.3-2008 is simulated.
The test pieces provided in examples 1 to 20 and comparative examples 1 to 10 were hung in an experimental apparatus, the temperature of the experimental apparatus was adjusted to 50. + -. 1 ℃ and pH was adjusted to 3.0 to 3.1, and then NaCl solution having a concentration of 5. + -. 0.5% was continuously sprayed to the test pieces. Taking example 1 and comparative example 10 as examples, after 8h, 24h, 48h and 72h of NaCl solution with the concentration of 5 +/-0.5% is sprayed on the test piece continuously, the weight loss rate of the test piece is shown in figure 3 (in figure 3, (A) represents comparative example 10, (B) represents example 1), and the specific experimental results of examples 1-20 and comparative examples 1-10 are shown in table 4.
It can be found by combining fig. 3 that the A, B test pieces have significantly different corrosion laws, and for the a test piece, the corrosion weight loss value tends to increase with the increase of the corrosion time. In the initial stage of corrosion (8-24h), an oxide film exists on the surface of the sample, so that the contact of a zirconium alloy matrix and a solution is prevented, and the corrosion rate is low. In the middle stage of corrosion (24-48h), Cl in the solution-Has penetrated the oxide film and has a large amount of Cl-The corrosion inhibitor is adsorbed on a substrate, so that pitting pits are increased, original pitting pits are deepened, and the corrosion rate is obviously accelerated. After 48h of continuous spraying, the corrosion products were distributed uniformly and increased in thickness, covering almost the entire surface of the test specimen, with Cl-The need to penetrate the corrosion products to contact the zirconium alloy substrate reduces the adsorption of Cl on the substrate surface-In such an amount that the corrosion rate is reduced. In general, the corrosion weight loss of the A test piece is far higher than that of the B test piece,the B test piece was substantially free from corrosion due to the presence of the coating, and its quality hardly changed. Therefore, the ultra-limit zirconium alloy provided by the application has better corrosion resistance.
The results of the experiment are shown in table 4: (A, stable creep time (min) of each test piece at 50MPa and 2000 ℃, creep rupture time (min) of each test piece at B, 50MPa and 2000 ℃, and C, weight loss rate (v/mg. cm) of each test piece after NaCl solution is continuously sprayed on the test pieces for 8 hours2) (ii) a D. And (3) continuously spraying NaCl solution to the test piece for 24 hours to obtain the weight loss ratio (v/mg2) (ii) a E. And (3) continuously spraying NaCl solution to the test piece for 48 hours to obtain the weight loss ratio (v/mg2) (ii) a F. And (3) continuously spraying NaCl solution to the test piece for 72 hours to obtain the weight loss ratio (v/mg2))
TABLE 4
Figure GDA0002293991000000171
Figure GDA0002293991000000181
In conclusion, the ultra-limit zirconium alloy prepared by the preparation method of the ultra-limit zirconium alloy provided by the invention has the advantages of wide use temperature range and strong corrosion resistance, and the best effect is obtained in example 1. The maximum service temperature of the zirconium alloy which is beyond the parameter range provided by the embodiment is much lower than that of the ultra-limit zirconium alloy provided by the invention, and the corrosion resistance of the zirconium alloy is poor.
It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention, and these changes and modifications should not be construed as affecting the performance of the invention and its practical application.

Claims (3)

1. A super-limit zirconium alloy comprises a zirconium alloy matrix and is characterized in that: the surface of the zirconium alloy substrate is sequentially deposited with a bonding layer, a noble metal layer, a ceramic A layer and a ceramic B layer, and the surface of the ceramic B layer is also sequentially deposited with a sealing coating, a reflecting layer and a reflecting layerA refractive layer and an electrically insulating layer; the thickness of the bonding layer is 50-150 mu m, the thickness of the noble metal layer is 10-20 mu m, the thickness of the ceramic layer A is 50-80 mu m, the thickness of the ceramic layer B is 50-80 mu m, the thickness of the sealing coating layer is 5-10 mu m, the thickness of the reflecting layer is 10-15 mu m, the thickness of the catadioptric layer is 10-15 mu m, and the thickness of the electric insulating layer is 15-20 mu m; the bonding layer comprises MCrAlY, wherein the MCrAlY is CoCrAlY, NiCoCrAlY or CoNiCrAlY; the component of the noble metal layer is one or more of Pt, Ru, Rh, Pd, Ir and Os alloy; the composition of the ceramic A layer is Y2O3-ZrO2、Y2O3-CeO2、Y2O3-TiO2、Y2O3-Yb2O3、Y2O3-Er2O3、Y2O3-Dy2O3、Y2O3-HfO2One or a mixture of several of them; the ceramic B layer is RETaO4，RETaO4Is spherical and has a particle size of 10-70 μm; the component of the sealing coating is Ti3SiC、REPO4And BN, or a mixture of more than one of them; the composition of the reflecting layer is REVO4、RETaO4、Y2O3One or a mixture of several of them; the component of the catadioptric layer is graphene, and the spatial distribution of the graphene is in a disordered arrangement state; the electric insulating layer is composed of one or a mixture of more of polytetrafluoroethylene, polyimide, polyphenyl ether, polyphenylene sulfide, polyether ether ketone, bismaleimide, furan resin, cyanate resin and polyarylethynyl.
2. The method for preparing the ultra-limit zirconium alloy according to claim 1, comprising the following steps:
the method comprises the following steps:
depositing a 50-150 mu m thick bonding layer on the surface of the zirconium alloy substrate by using an HVOF method;
step two:
depositing a noble metal layer with the thickness of 10-20 microns on the surface of the bonding layer by using an HVOF method;
step three:
depositing a ceramic A layer with the thickness of 50-80 microns on the surface of the noble metal by using a plasma spraying technology;
step four:
depositing a 50-80 mu m thick ceramic layer B on the surface of the ceramic layer A by using a plasma spraying technology;
step five:
depositing a sealing coating layer with the thickness of 5-10 mu m on the surface of the ceramic B layer by using an electron beam physical vapor deposition technology;
step six:
depositing a reflecting layer with the thickness of 10-15 microns on the surface of the sealing coating by using an electron beam physical vapor deposition technology;
step seven:
depositing a 10-15 mu m-thick catadioptric layer on the surface of the reflecting layer by using a brushing method;
step eight:
adhering materials by using sponge, vibrating the sponge by using a vibration polishing machine, and depositing an electric insulation layer with the thickness of 15-20 microns on the surface of the catadioptric layer so as to prepare the ultra-limit zirconium alloy.
3. The method for preparing the ultra-limit zirconium alloy according to claim 2, wherein: in the first step, before the bonding layer is deposited, oil stains on the surface of the zirconium alloy substrate are removed; and performing sand blasting treatment on the surface of the zirconium alloy matrix to ensure that the surface roughness of the zirconium alloy matrix is 60-100 mu m.
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