CN109609952B - Ultra-limit magnesium alloy and preparation method thereof - Google Patents
Ultra-limit magnesium alloy and preparation method thereof Download PDFInfo
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- CN109609952B CN109609952B CN201811640744.4A CN201811640744A CN109609952B CN 109609952 B CN109609952 B CN 109609952B CN 201811640744 A CN201811640744 A CN 201811640744A CN 109609952 B CN109609952 B CN 109609952B
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Abstract
The invention belongs to the technical field of magnesium alloy metal materials, and discloses an ultra-limit magnesium alloy and a preparation method thereof, wherein the ultra-limit magnesium alloy comprises a magnesium alloy matrix, wherein an antioxidant composite bonding layer, a composite ceramic layer, a reflecting layer, an anti-refraction layer, an insulating layer and a foam carbon layer are sequentially deposited on the surface of the magnesium alloy matrix; the anti-oxidation composite bonding layer comprises a bonding layer deposited on the surface of the magnesium alloy substrate and a noble metal layer deposited on the surface of the bonding layer; the composite ceramic layer comprises a ceramic A layer and a ceramic B layer. During preparation, the anti-oxidation composite bonding layer, the composite ceramic layer, the reflecting layer, the anti-refraction layer, the insulating layer and the foam carbon layer are deposited on the surface of the magnesium alloy in sequence, so that the ultra-limit magnesium alloy is formed. The use temperature of the super-limit magnesium alloy provided by the invention is increased to be higher than the melting point of the original magnesium alloy by 100-500 ℃, and the super-limit magnesium alloy can be used at the super-limit temperature.
Description
Technical Field
The invention belongs to the field of magnesium alloy metal materials, and particularly relates to an ultra-limit magnesium alloy and a preparation method thereof.
Background
Magnesium alloys, an important metal material today, have a low density (1.8 g/cm)3Left and right), high strength, large elastic modulus, good heat dissipation, good shock absorption, and impact resistanceThe load capacity is larger, the corrosion resistance of organic matters and alkali is good, and the like, and the material is mainly used for aviation, aerospace, transportation, chemical engineering, rockets and other industrial departments. Magnesium alloys are the lightest metallic structural materials used in the aircraft, spacecraft and rocket missile manufacturing industries, and are mainly used for manufacturing parts with low bearing capacity.
With the development of technology and the practical requirements of society, the speed requirement on the aircraft is higher and higher, the speed increase of the aircraft means that the running speed of the engine is increased, and the running temperature of the engine is increased, so that the temperatures of a gear case, an oil pump, an oil pipe and the like of the engine are also increased. Whereas magnesium alloys are stable in gasoline, kerosene and lubricating oil, and therefore engine gear housings, oil pumps and oil pipes are generally prepared from magnesium alloys. The magnesium alloy of the magnesium alloy has a melting point of about 650 ℃, the use temperature of about 70% of the melting point of the magnesium alloy, and the magnesium alloy is very easy to oxidize at high temperature, so that when the aircraft accelerates, the magnesium alloy can not be used under the condition that the temperature of each part of an engine is increased, and therefore the magnesium alloy can be used at the ultra-limit temperature (the ultra-limit temperature is the temperature exceeding the melting point of the magnesium alloy).
In the research process of increasing the flight speed of the aircraft, in order to adapt to the increase of the temperature of the engine of the aircraft, the alloy with a higher melting point, such as iron alloy, is generally used as a main structural material for manufacturing the aircraft, but the weight of the iron alloy is larger, and the use of the iron alloy as a raw material for manufacturing the engine of the aircraft can cause the weight of the engine of the aircraft to be greatly increased, but can cause the flight speed of the aircraft to be reduced, so that the actual requirement cannot be met. If the aircraft is accelerated without changing the material, the service life of the aircraft can be shortened.
Disclosure of Invention
The invention aims to provide an ultra-limit magnesium alloy and a preparation method thereof, and aims to solve the problem that the magnesium alloy cannot be used at an ultra-limit temperature.
In order to achieve the aim, the invention provides the following basic scheme that the ultra-limit magnesium alloy comprises a magnesium alloy matrix, wherein an anti-oxidation composite bonding layer and a composite ceramic layer are sequentially deposited on the surface of the magnesium alloy matrix; the anti-oxidation composite bonding layer comprises a bonding layer deposited on the surface of the magnesium alloy substrate and a noble metal layer deposited on the surface of the bonding layer; the composite ceramic layer comprises a ceramic A layer and a ceramic B layer.
The beneficial effects of the technical scheme are as follows:
through a great deal of research, the inventor develops a super-limit magnesium alloy which meets the requirement that the magnesium alloy is used at a super-limit temperature (exceeding the melting point temperature). In the development process, people generally consider that when the ambient temperature is higher than the use temperature of the alloy, the alloy cannot be used at the temperature, and other high-melting-point alloys are required to be used, and the inventors try to improve the magnesium alloy to meet the requirements of aircraft manufacturing. In the process of continuous trial by the inventor, the inventor discovers that the use temperature of the magnesium alloy can be increased to be higher than the original melting point by 100-500 ℃ by depositing a coating with a certain proportion on the surface of the magnesium alloy, so that the use temperature of the magnesium alloy can be greatly increased, and the requirement of manufacturing an aircraft can be met; in a high-temperature environment, the use temperature of the magnesium alloy is difficult to be raised by 2-3 ℃, so that the research of the applicant is a great progress on the use of the magnesium alloy.
According to the technical scheme, the anti-oxidation composite bonding layer and the composite ceramic layer are deposited on the magnesium alloy substrate, so that the use temperature of the magnesium alloy can be greatly increased, and the magnesium alloy is suitable for being used at the ultra-limit temperature. The anti-oxidation composite bonding layer is deposited, so that the bonding effect between each coating and the magnesium alloy matrix can be improved, and the coating is prevented from falling off in the using process. The composite ceramic layer is deposited, so that the heat conduction can be reduced, and the service temperature of the magnesium alloy matrix can be increased.
In summary, the present invention has the following technical effects:
1. the ultra-limit magnesium alloy provided by the invention has excellent high-temperature mechanical and chemical stability, can be used under the condition of exceeding the melting point of a magnesium alloy matrix, and enhances the application range.
2. According to the invention, the multilayer coating is deposited on the surface of the magnesium alloy substrate, so that the use temperature of the magnesium alloy substrate can be raised to be higher than the melting point of the original magnesium alloy substrate by 100-.
3. The ultra-limit magnesium 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 method breaks through the limitation of the traditional idea that only the material can be replaced when the environmental temperature is higher than the use temperature of the material, and improves the use temperature of the material by depositing the coating on the surface of the material, so that the ultra-limit magnesium alloy can be suitable for the preparation of the accelerated aircraft, and the service life of the aircraft cannot be shortened.
Further, the thickness of the anti-oxidation composite bonding layer is 100-200 mu m, the thickness of the composite ceramic layer is 150-500 mu m, and a reflecting layer with the thickness of 10-30 mu m, an anti-refraction layer with the thickness of 10-30 mu m, an insulating layer with the thickness of 10-200 mu m and a foam carbon layer with the thickness of 20-200 mu m are sequentially deposited outside the composite ceramic layer.
Has the advantages that: the deposited reflecting layer has the effect of reflecting a heat source, so that the heat source on the surface of the magnesium alloy is reduced, and the use temperature is increased. The anti-refraction layer is deposited, so that the refraction of infrared rays in the coating can be blocked, the temperature of the magnesium alloy matrix is reduced, and the service temperature of the prepared magnesium alloy is increased. The insulating layer can isolate the ionization generation on the surface of the magnesium alloy substrate and resist the erosion of charges to the substrate material. When in use, the carbon of the foam carbon layer is vaporized and cooled, and a vaporization film is formed on the surface of the magnesium alloy substrate, so that the heat transmission is further prevented, and the use temperature of the magnesium alloy is increased. According to the technical scheme, the service temperature of the magnesium alloy is greatly improved through the matching of the coatings. And the thickness of each coating is set, so that the service temperature of the prepared ultra-limit magnesium alloy is improved, the weight increase is less, the characteristic of light weight is realized, and the aircraft is convenient to manufacture and use.
Furthermore, the bonding layer comprises one or a mixture of more of MCrAlY, NiAl, NiCr-Al and Mo, wherein the MCrAlY is NiCrCoAlY, NiCoCrAlY, CoNiCrAlY or CoCrAlY; the component of the noble metal layer is one or more of Au, Pt, Ru, Rh, Pd and Ir.
Has the advantages that: the proportions of elements in the three materials of NiCrCoAlY, NiCoCrAlY and CoNiCrAlY are 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 magnesium 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 magnesium 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 ceramic A layer contains YSZ or rare earth zirconate (RE)2Zr2O7) (ii) a The component of the ceramic B layer is ZrO2-RETaO4。
Has the advantages that: YSZ or rare earth zirconate, a commonly used material as a thermal barrier coating, is readily available. ZrO (ZrO)2-RETaO4The magnesium alloy has the characteristics of low thermal conductivity and high expansion, and the low thermal conductivity can reduce the conduction of heat, so that the magnesium alloy matrix keeps low temperature in a high-temperature environment, and the service temperature of the prepared magnesium alloy is improved; 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 ZrO2-RETaO4Is spherical and has a particle size of 10-70 μm.
Has the advantages that: when the ceramic B layer is deposited, the spraying effect is good, and the bonding effect of the ceramic B layer is good.
Further, the reflective layer has a composition of REVO4、RETaO4、Y2O3One or a mixture of several of them.
Has the advantages that: REVO4、RETaO4And the reflection coefficient of Y2O3 is high, so that the heat source can be reflected, the heat radiation is reduced, the temperature of the magnesium alloy matrix is reduced, and the service temperature of the prepared magnesium alloy is increased.
Furthermore, the ingredient of the anti-refraction layer is one or a mixture of two of graphene and boron carbide, and the crystal structures of the graphene and the boron carbide are in a disordered arrangement state.
Has the advantages that: although the graphene and the boron carbide have higher refractive indexes, when incident light irradiates on the anti-refraction layer, the graphene and the boron carbide which are arranged in an unordered mode 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 insulating layer is made of one or a mixture of epoxy resin, phenolic resin and ABS resin.
Has the advantages that: when the aircraft is used, the shell is rubbed with air and ionized, and the epoxy resin, the phenolic resin and the ABS resin can isolate conductive electrons and resist the corrosion of charges on a magnesium alloy matrix.
The invention also provides another basic scheme, and the preparation method of the ultra-limit magnesium alloy comprises the following steps:
the method comprises the following steps:
firstly, depositing a bonding layer on the surface of a magnesium alloy substrate, and then depositing a noble metal layer on the surface of the bonding layer, so that the bonding layer and the noble metal layer form an antioxidant composite bonding layer, wherein the total thickness of the antioxidant composite bonding layer is 100-200 mu m;
step two:
depositing a ceramic layer A and a ceramic layer B on the surface of the noble metal layer to form a composite ceramic layer, wherein the total thickness of the composite ceramic layer is 150-500 mu m;
step three:
depositing a reflecting layer on the surface of the composite ceramic layer, wherein the thickness of the reflecting layer is 10-30 mu m;
step four:
coating an anti-refraction layer on the surface of the reflecting layer, wherein the thickness of the anti-refraction layer is 10-30 mu m;
step five:
coating an insulating layer on the surface of the anti-refraction layer, wherein the thickness of the insulating layer is 10-200 mu m;
step six:
and coating a foamed carbon layer on the surface of the insulating layer, wherein the thickness of the foamed carbon layer is 20-200 mu m, so that the ultra-limit magnesium alloy is formed.
The beneficial effects of this technical scheme do:
by controlling the thickness of each coating deposited on the magnesium alloy substrate, the service temperature of the prepared ultra-limit magnesium alloy can be increased to 100-500 ℃ higher than the melting point of the original magnesium alloy, and the magnesium alloy has excellent corrosion resistance. Meanwhile, the situation that the weight of the prepared ultra-limit magnesium alloy is increased greatly due to the fact that the thickness of the coating is large can be avoided, so that the ultra-limit magnesium alloy can keep the light characteristic and can be used at the ultra-limit temperature, and the use requirement of the existing aircraft for speed increase is met.
Further, in the first step, before the bonding layer is deposited, oil stains on the surface of the magnesium alloy substrate are removed; and shot blasting the surface of the magnesium alloy matrix to ensure that the surface roughness of the magnesium alloy matrix is 60-100 mu m.
Has the advantages that: the bonding effect between the magnesium alloy matrix and the coating can be improved by removing the oil stain on the surface of the magnesium alloy matrix. And the coating can generate larger internal stress in the process of curing, and the problem of stress concentration can be effectively solved by utilizing the roughness of the surface of the magnesium alloy substrate subjected to shot blasting treatment by a shot 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 view of an ultra-limited magnesium alloy according to the present invention;
FIG. 2 is a graph showing creep tests at 900 ℃ under 50MPa in example 1 of the present invention and in comparative example 13;
FIG. 3 is a graph showing the results of the salt spray corrosion test in example 1 of the present invention and comparative example 13.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the magnesium alloy substrate comprises a magnesium alloy substrate 1, an antioxidant composite bonding layer 2, a bonding layer 21, a noble metal layer 22, a composite ceramic layer 3, a ceramic A layer 31, a ceramic B layer 32, a reflecting layer 4, an anti-refraction layer 5, an insulating layer 6 and a foam carbon layer 7.
The invention provides a super-limit magnesium alloy, which comprises a magnesium alloy substrate 1, wherein an antioxidant composite bonding layer 2 with the thickness of 100-200 mu m, a composite ceramic layer 3 with the thickness of 150-500 mu m, a reflecting layer 4 with the thickness of 10-30 mu m, an anti-refraction layer 5 with the thickness of 10-30 mu m, an insulating layer 6 with the thickness of 10-200 mu m and a foam carbon layer 7 with the thickness of 20-200 mu m are sequentially deposited on the surface of the magnesium alloy substrate 1 as shown in figure 1. The anti-oxidation composite bonding layer 2 comprises a bonding layer 21 deposited on the surface of the magnesium alloy substrate 1 and a precious metal layer 22 deposited on the surface of the bonding layer 21, the bonding layer 21 is made of one or more of MCrAlY, NiAl, NiCr-Al and Mo, MCrAlY is NiCrCoAlY, NiCoCrAlY, CoNiCrAlY or CoCrAlY, and the precious metal layer 22 is made of one or more of Au, Pt, Ru, Rh, Pd and Ir; the composite ceramic layer 3 comprises a ceramic A layer 31 and a ceramic B layer 32, the ceramic A layer 31 is close to the noble metal layer 22 or the ceramic B layer 32 is close to the noble metal layer 22, and the ceramic A layer 31 is composed of YSZ or rare earth zirconate (RE)2Zr2O7RE ═ Y, Nd, Eu, Gd, Dy, Sm), the component of the ceramic B layer 32 is ZrO2-RETaO4，ZrO2-RETaO4Is spherical, has a particle diameter of 10-70 μm and has a chemical formula of RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4RE ═ Y, Nd, Eu, Gd, Dy, Er, Yb, Lu, Sm; the reflective layer 4 has a composition of REVO4、RETaO4、Y2O3One or more of RE, Y, Nd, Eu, Gd, Dy, Er, Yb, Lu and Sm. The ingredient of the anti-refraction layer 5 is one or a mixture of two of graphene and boron carbide, and the crystal structures of the graphene and the boron carbide are in a disordered arrangement state; insulating layer 6The component (A) is one or a mixture of more of epoxy resin, phenolic resin and ABS resin.
The invention utilizes ZrO2-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 ZrO prepared by the following method2-RETaO4Can meet the requirements of APS spraying technology.
ZrO2-RETaO4The preparation method comprises the following steps:
step (1):
zirconium oxide (ZrO)2) Powder, rare earth oxide powder (RE)2O3) Tantalum pentoxide (Ta)2O5) Pre-drying the powder at 600 ℃ for 8 h; and in a molar ratio of 2 x: (1-x): (1-x) weighing zirconium oxide (ZrO)2) Powder, rare earth oxide powder RE2O3Tantalum oxide (Ta)2O5) Adding the powder into an ethanol solvent to obtain a mixed solution, wherein the molar ratio of RE to Ta to Zr in the mixed solution is (1-x) to 2 x; 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 ZrO from the powder A obtained in the step (1) by adopting a high-temperature solid-phase reaction method2Doped RETaO4The 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 ZrO with particle size of 10-70 nm2-RETaO4Ceramic powder.
The inventor finds out through a large number of experiments that the service temperature of the prepared ultra-limit magnesium alloy is increased most within the parameter range of the invention, the weight increment of the magnesium alloy is small, and the ultra-limit magnesium alloy with the optimal parameter range is provided, and 30 groups are listed for description in the invention.
The parameters of examples 1 to 30 of the ultra-limited magnesium alloy and the preparation method thereof of the present invention are shown in tables 1, 2 and 3: (thickness unit: μm)
TABLE 1
TABLE 2
TABLE 3
Now, a method for preparing an ultra-limited magnesium alloy according to another embodiment of the present invention will be described with reference to example 1.
A preparation method of an ultra-limit magnesium alloy comprises the following steps:
the method comprises the following steps:
in this example, AM50A magnesium alloy is selected as the magnesium alloy substrate, and the immersion method is used to remove oil stain and impurities on the surface of the magnesium alloy substrate, the magnesium alloy substrate is first immersed in an emulsion cleaning solution or an alkali solution, wherein the main components of the emulsion cleaning solution are ethanol and a surfactant, and the main components of the alkali solution are sodium hydroxide, trisodium phosphate and sodium carbonate sodium silicate, and the magnesium alloy substrate is immersed in the alkali solution in this example. Adjusting the pH value of the alkali solution to 10-11, soaking the magnesium alloy substrate in the alkali solution for 0.5-1.5h, taking out the magnesium alloy substrate, wherein the soaking time is 1h in the embodiment, and then washing the magnesium alloy substrate with clear water and drying the magnesium alloy substrate. Performing shot blasting treatment on the surface of the magnesium alloy substrate by using a shot blasting machine, wherein the used shot blasting machine is a JCK-SS500-6A automatic transmission type shot blasting machine, the shot blasting material adopted in shot blasting is any one of iron sand, glass shot and ceramic shot, the iron sand is used in the embodiment, the particle size of the iron sand can be 0.3-0.8mm, and the particle size of the iron sand in the embodiment is 0.5 mm; the surface roughness of the magnesium alloy matrix after shot blasting is 60-100 μm, and the surface roughness of the magnesium alloy matrix in the embodiment is 80 μm, so that the coating and the magnesium alloy matrix can be conveniently bonded.
Step two:
an oxidation resistant composite bonding layer is deposited on the surface of AM50A magnesium alloy after shot blasting, firstly, a NiCrCoAlY layer is sprayed on the surface of a magnesium alloy substrate by HVOF or supersonic electric arc spraying method to be used as the bonding layer, in the embodiment, the HVOF method is used, the powder grain size is 25-65 μm, the oxygen flow is 2000SCFH, the kerosene flow is 18.17LPH, the carrier gas is 12.2SCFH, the powder feeding amount is 5RPM, the gun barrel length is 5in, and the spraying distance is 254 mm.
And depositing a layer of Au as a noble metal layer on the NiCrCoAlY by using an EB-PVD method so as to form the oxidation-resistant composite bonding layer. The gas pressure when depositing Au is less than 0.01Pa, the pressure used in the embodiment is 0.008Pa, and the ratio of the temperature of the magnesium alloy substrate to the melting point of the magnesium alloy substrate is less than 0.3. The thickness of the deposited bonding layer was 50 μm and the thickness of the noble metal layer was 50 μm.
Step three:
spraying a layer of YSZ on the surface of the bonding layer as a ceramic A layer by using APS, HVOF, PS-PVD or EB-PVD method, wherein APS method is used in the embodiment, and then spraying a layer of YTaO on the ceramic A layer by using APS method4Forming a composite ceramic layer as a ceramic layer B; wherein the thickness of the ceramic A layer is 70 μm and the thickness of the ceramic B layer is 80 μm.
Step four:
spraying a layer of Y on the surface of the B layer of the ceramic by using HVOF, PS-PVD or EB-PVD method2O3The transparent ceramic material was used as a reflective layer, and the thickness of the reflective layer sprayed was 10 μm in this example using the HVOF method.
Step five:
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 then coating the solution mixed with the graphene on the surface of the reflecting layer to serve as an anti-refraction layer, putting the magnesium alloy coated with the graphene anti-refraction layer into a drying box, and drying at the temperature of 60 ℃ for 2 hours, wherein the thickness of the coated anti-refraction layer is 10 microns.
Step six:
and coating a layer of epoxy resin on the surface of the anti-refraction layer to be used as an insulating layer, wherein the thickness of the insulating layer is 10 mu m.
Step seven:
and coating a foam carbon layer on the insulating layer, wherein the thickness of the foam carbon layer is 20 mu m, and the ultra-limit magnesium alloy is obtained.
Examples 2-29 differed from example 1 only in the parameters shown in table 1; example 30 differs from example 1 in the spraying sequence of the ceramic a and B layers in step three.
Experiment:
set up 13 sets of comparative experiments with the comparative examples 1-30, the parameters of comparative examples 1-12 are shown in table 4:
TABLE 4
Comparative examples 1 to 12 are different from example 1 only in the respective parameters shown in table 3, and comparative example 13 is AM50A magnesium alloy.
The following experiments were carried out using the magnesium alloys provided in examples 1 to 30 and comparative examples 1 to 13:
high temperature creep test:
the magnesium alloys provided in examples 1 to 30 and comparative examples 1 to 13 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 30 and comparative examples 1 to 13 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 900 ℃, the testing machine was adjusted to a stress of 50MPa, and a high temperature creep test was conducted, taking example 1 and comparative example 13 as examples, the test results are shown in fig. 2 (a) shows comparative example 13, (B) shows example 1), and the specific test results of examples 1 to 30 and comparative examples 1 to 13 are shown in table 5.
As can be seen from fig. 2, the (a) and (B) test pieces had 3 stages of creep, but at a temperature after exceeding the melting point of the AM50A magnesium alloy, the (a) test piece had creep rupture in an extremely short time, and therefore, it can be seen that the AM50A magnesium alloy was hardly loaded at a temperature higher than the melting point of the AM50A magnesium 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 AM50A magnesium alloy, the ultra-limit magnesium alloy provided by the invention has the advantages that the ultra-limit magnesium alloy keeps better mechanical property without cracking and has excellent high-temperature resistance at the temperature exceeding the melting point of the AM50A magnesium alloy.
Salt spray corrosion test:
the magnesium alloys provided in examples 1 to 30 and comparative examples 1 to 13 were processed into test pieces of 50mm × 25mm × 2mm, and then subjected to oil removal and rust removal treatment, and then cleaned and dried. 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 30 and comparative examples 1 to 13 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 NaCl solution having a concentration of 5. + -. 0.5% was continuously sprayed to the test pieces. Taking example 1 and comparative example 13 as examples, after spraying NaCl solution with concentration of 5 +/-0.5% for 8h, 24h, 48h and 72h continuously to the test piece, the weight loss rate of the test piece is shown in FIG. 3 (A) represents comparative example 13, (B) represents example 1), and the specific experimental results of examples 1-30 and comparative examples 1-13 are shown in Table 5.
The combination of FIG. 3 shows that the (A) and (B) test pieces have obviously different corrosion rules, and the corrosion weight loss value of the (A) test piece is increased along with the prolonging of the corrosion timeA large trend. In the initial stage of corrosion (8-24h), an oxide film exists on the surface of the sample, so that the magnesium alloy substrate is prevented from contacting with the solution, 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-Needs to penetrate through corrosion products to be contacted with the magnesium alloy substrate, thereby reducing the Cl adsorption on the surface of the substrate-In such an amount that the corrosion rate is reduced. In general, (A) the corrosion weight loss of the test piece is far higher than that of the test piece (B), and the quality of the test piece (B) is hardly changed because the coating is basically corroded, so that the ultra-limit magnesium alloy provided by the application has better corrosion resistance.
The results of the experiment are shown in table 5: (A, stable creep time (min) of each test piece at 50MPa and 900 ℃, creep rupture time (min) of each test piece at B, 50MPa and 900 ℃, and weight loss rate (v/mg. cm) of each test piece after NaCl solution is continuously sprayed on the test piece for 8 hours2) (ii) a B. 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 5
Therefore, the anti-oxidation composite bonding layer, the composite ceramic layer, the reflecting layer, the anti-refraction layer, the insulating layer and the foam carbon layer are deposited on the magnesium alloy, so that the service temperature of the magnesium alloy can be increased to be higher than the original melting point of 100-500 ℃, and the corrosion resistance is also greatly improved. And the thickness of each coating is controlled within the range provided by the invention, so that each effect of the prepared ultra-limit magnesium alloy can be optimal. The maximum service temperature of the magnesium alloy beyond the parameter range provided by the embodiment is much lower than that of the ultra-limit magnesium alloy provided by the invention, and the corrosion resistance of the magnesium 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 (4)
1. An ultra-limit magnesium alloy comprises a magnesium alloy matrix and is characterized in that: an anti-oxidation composite bonding layer and a composite ceramic layer are sequentially deposited on the surface of the magnesium alloy substrate; the anti-oxidation composite bonding layer comprises a bonding layer deposited on the surface of the magnesium alloy substrate and a noble metal layer deposited on the surface of the bonding layer; the composite ceramic layer comprises a ceramic layer A and a ceramic layer B; a reflecting layer, an anti-refraction layer, an insulating layer and a foam carbon layer are sequentially deposited outside the composite ceramic layer; the thickness of the anti-oxidation composite bonding layer is 100-200 mu m, the thickness of the composite ceramic layer is 150-500 mu m, the thickness of the reflecting layer is 10-30 mu m, the thickness of the anti-refraction layer is 10-30 mu m, the thickness of the insulating layer is 10-200 mu m and the thickness of the foam carbon layer is 20-200 mu m; the bonding layer is made of one or a mixture of more of MCrAlY, NiAl, NiCr-Al and Mo, and the MCrAlY is NiCrCoAlY, NiCoCrAlY, CoNiCrAlY or CoCrAlY; the component of the noble metal layer is one or more of Au, Pt, Ru, Rh, Pd and Ir; the ceramic layer A contains YSZ or rare earth zirconate (RE)2Zr2O7) (ii) a The component of the ceramic B layer is ZrO2-RETaO4(ii) a The composition of the reflecting layer is REVO4、RETaO4、Y2O3One or a mixture of several of them; the component of the anti-refraction layer is one or a mixture of two of graphene or boron carbide, and the crystal structures of the graphene and the boron carbide are in a disordered arrangement state; the insulating layer is composed of one or a mixture of more of epoxy resin, phenolic resin and ABS resin.
2. According to claim 1The ultra-limit magnesium alloy is characterized in that: the ZrO2-RETaO4Is spherical and has a particle size of 10-70 μm.
3. The method for preparing the ultra-limit magnesium alloy according to the claim 1 or 2, characterized by comprising the following steps:
the method comprises the following steps:
firstly, depositing a bonding layer on the surface of a magnesium alloy substrate by using an HVOF or supersonic electric arc spraying method, and then depositing a noble metal layer on the surface of the bonding layer by using an EB-PVD method, so that the bonding layer and the noble metal layer form an antioxidant composite bonding layer, wherein the total thickness of the antioxidant composite bonding layer is 100-200 mu m;
step two:
depositing a ceramic layer A and a ceramic layer B on the surface of the noble metal layer by using an APS (advanced passivation solution), HVOF (high voltage oxygen gas), PS-PVD (PS-physical vapor deposition) or EB-PVD (electron beam physical vapor deposition) method, so that the ceramic layer A and the ceramic layer B form a composite ceramic layer, wherein the total thickness of the composite ceramic layer is 150-500 mu m;
step three:
depositing a reflecting layer on the surface of the composite ceramic layer by using an HVOF, PS-PVD or EB-PVD method, wherein the thickness of the reflecting layer is 10-30 mu m;
step four:
coating an anti-refraction layer on the surface of the reflecting layer by a coating method, wherein the thickness of the anti-refraction layer is 10-30 mu m;
step five:
coating an insulating layer on the surface of the anti-refraction layer by a coating method, wherein the thickness of the insulating layer is 10-200 mu m;
step six:
and (3) coating a foamed carbon layer on the surface of the insulating layer by using a coating method, wherein the thickness of the foamed carbon layer is 20-200 mu m, so that the ultra-limit magnesium alloy is formed.
4. The method for preparing the ultra-limit magnesium alloy according to claim 3, wherein the method comprises the following steps: in the first step, before the bonding layer is deposited, oil stains on the surface of the magnesium alloy substrate are removed; and shot blasting the surface of the magnesium alloy matrix to ensure that the surface roughness of the magnesium alloy matrix is 60-100 mu m.
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| CN201811640744.4A CN109609952B (en) | 2018-12-29 | 2018-12-29 | Ultra-limit magnesium alloy and preparation method thereof |
| EP19903063.6A EP3904555A4 (en) | 2018-12-29 | 2019-11-12 | Ultralimit alloy and preparation method therefor |
| US17/419,250 US11530485B2 (en) | 2018-12-29 | 2019-11-12 | Ultralimit alloy and preparation method therefor |
| JP2021538453A JP7242867B2 (en) | 2018-12-29 | 2019-11-12 | Superalloy and its manufacturing method |
| PCT/CN2019/117283 WO2020134655A1 (en) | 2018-12-29 | 2019-11-12 | Ultralimit alloy and preparation method therefor |
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