CN105834435B - Wet mixing preparation method of nickel-based high-temperature olefin alloy powder - Google Patents
Wet mixing preparation method of nickel-based high-temperature olefin alloy powder Download PDFInfo
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- CN105834435B CN105834435B CN201511021007.2A CN201511021007A CN105834435B CN 105834435 B CN105834435 B CN 105834435B CN 201511021007 A CN201511021007 A CN 201511021007A CN 105834435 B CN105834435 B CN 105834435B
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Abstract
The invention provides a preparation method of nickel-based high-temperature alkene alloy powder. Firstly, selecting a graphene oxide sheet to be dissolved in water to prepare a graphene oxide solution with a certain content; then adding high-temperature alloy powder prepared by an argon atomization method (AA) or a plasma rotating electrode method (PREP) into the graphene oxide solution, and ultrasonically vibrating and stirring to disperse graphene oxide sheets on the surface of high-temperature alloy powder particles; washing and filtering the mixed graphene oxide/high-temperature alloy powder, and drying the graphene oxide/high-temperature alloy powder in an oven; and finally, filling the dried graphene oxide/high-temperature alloy powder into a stainless steel sheath, and performing vacuum degassing and heating to prepare the graphene/high-temperature alloy composite powder.
Description
Technical Field
The invention relates to a preparation method of alloy powder, in particular to a preparation method of nickel-based high-temperature alkene alloy powder.
Background
With the further demands of the aviation industry for material properties, nickel-based composites are also widely developed and used. In recent decades, research on carbon materials has been a focus of research at the scientific frontier. Research on carbon materials as reinforcements for nickel-based superalloy composites is increasing. Graphene, one of the most tough, electrically and thermally conductive materials found so far, is known as a new generation of strategic material. The graphene has excellent characteristics of high carrier mobility, large current density, high strength, high thermal conductivity and the like, particularly excellent mechanical properties, which are 2-3 orders of magnitude higher than those of common metal materials, and Young modulus higher than 1GPa, so that the graphene has great potential in application and research of graphene composite materials. If the advantages of high strength, high specific modulus and the like of graphene and the advantages of high strength, high fatigue performance and the like of nickel-based powder superalloy can be combined, a graphene reinforced nickel-based composite material with excellent performance is expected to be developed. The problem of dispersibility between graphene and high-temperature alloy powder is firstly solved when the nickel-based high-temperature graphene alloy composite material is prepared. Due to the fact that graphene is low in density, poor in dispersity and large in property difference with a high-temperature alloy matrix, adding graphene into a metal material by a traditional smelting and metallurgy method is extremely difficult.
The method is found through relevant document retrieval at home and abroad: the poly (terephthalic acid) (PET)/graphene composite material is prepared by melt blending in Ningbo material technology of Chinese academy of sciences and engineering research institute, and research shows that the conductivity of the composite material is greatly improved by adding graphene, and the conductivity of the composite material containing 3.0 vol% of graphene can reach 2.11S/m. Kuila et al, North China university, Korea, studied the mechanical properties of functionalized graphene vinyl acetate (EVA) copolymer composites, made up of Octadecylamine (ODA) as the surface modifier of graphene, and then blended with EVA to make copolymer composites with tensile strength increased by 74% and thermal stability increased by 42 ℃. Ramanathan and the like adopt a solution dispersion method to compound the modified graphene and polymethyl methacrylate (PMMA), and the thermodynamic property and the rheological property of the graphene are represented. They found that the elastic modulus of the modified graphene/PMMA composite material was increased by 30% and the hardness was increased by 5% compared to pure PMMA. However, these methods are applicable to the mixing between graphene and some polymer materials to improve the electrical conductivity, thermal stability and mechanical properties of the composite. Aiming at the method for preparing the graphene/high-temperature alloy composite powder by adding the graphene into the high-temperature alloy, the problems that the density difference between the high-temperature alloy and the graphene is large and the graphene is difficult to disperse are solved, and the prepared graphene/high-temperature alloy composite powder is subjected to a series of thermal technological processes such as thermal densification molding and the like, wherein the thermal technological temperatures are usually over 1000 ℃, and if the dispersion between the graphene and the high-temperature alloy powder is poor, the graphene/high-temperature alloy composite powder is easy to react with high-temperature alloy matrix elements at high temperature, so that the mechanical property of the alloy is influenced finally.
Disclosure of Invention
The invention provides a dispersion control method of graphene and high-temperature alloy powder, which is used for uniformly dispersing graphene nano-sheets in the high-temperature alloy powder. The advantages of high strength, high specific modulus and the like of the graphene nanosheets are combined with the nickel-based powder high-temperature alloy, so that the strengthening effect of the graphene sheets in the metal matrix is exerted, and the mechanical property of the material is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of nickel-based high-temperature alkene alloy powder comprises the following steps: 1) dissolving graphene oxide nanosheets in water or alcohol, performing ultrasonic stirring dispersion, standing the graphene oxide solution, and removing excess water or alcohol above the graphene oxide solution; 2) adding a small amount of nickel-based superalloy powder prepared by an AA method or a PREP method into a graphene oxide solution in batches, and continuously mechanically stirring; 3) repeatedly washing the mixed powder, and drying the powder in an oven to obtain graphene oxide/high-temperature alloy composite powder; 4) and then carrying out surface degassing treatment on the graphene oxide/high-temperature alloy powder, and filling the degassed mixed powder into a stainless steel sheath for sealing welding to prepare the graphene/high-temperature alloy composite powder.
According to the first preferable scheme of the preparation method of the nickel-based high-temperature graphene alloy powder, the graphene oxide nanosheets are prepared by adopting a redox method, a pyrolysis method or other methods, have a sheet structure with a single-layer thickness or a thickness of several atomic layers, and are less than 10nm in thickness.
According to the second priority scheme of the preparation method of the nickel-based high-temperature graphene alloy powder, the content of graphene oxide in a graphene oxide solution is 0.05-6 wt%; the ultrasonic stirring time is not less than 30 minutes, the stirring frequency is 2s of ultrasound, and the gap is 5 s.
According to the third preferred scheme of the preparation method of the nickel-based high-temperature graphene alloy powder, the standing time of the graphene oxide solution is 1-3 hours.
A fourth preferred embodiment of the method for preparing the nickel-based superalloy powder has a particle size of not greater than-200 mesh.
According to the fifth preferential scheme of the preparation method of the nickel-based high-temperature alkene alloy powder, the alloy powder is added in small quantities in batches, and the weight of the powder added in each batch is 200-1000 g.
In a sixth preferred embodiment of the method for producing a nickel-base superalloy powder, the mechanical stirring time is not less than 40 minutes.
According to a seventh preferred scheme of the preparation method of the nickel-based high-temperature alkene alloy powder, the composite powder is washed for 3-5 times.
An eighth preferred scheme of the preparation method of the nickel-based high-temperature alkene alloy powder is that the temperature of an oven is 50-100 ℃, and the drying time is 10-24 hours.
The ninth prior scheme of the preparation method of the nickel-based high-temperature alkene alloy powder is that the vacuum degree of degassing treatment is less than or equal to 5.0 multiplied by 10 < -3 > Pa, the degassing temperature is 200-400 ℃, and the degassing time is 3-12 h.
The excellent effects of the present invention compared to the closest prior art are as follows:
(1) the high-temperature alloy powder prepared by the AA method or the PREP method has finer and more uniform powder granularity and is beneficial to the dispersion between graphene nano sheets.
(2) Because the density of the high-temperature alloy powder is higher than that of common metal (magnesium, titanium, aluminum and the like) powder, and the difficulty of directly mixing the graphene powder and the high-temperature alloy powder is higher, the graphene is implanted into the high-temperature alloy powder by adopting a wet mixing method
(3) Considering that graphene is not hydrophilic or lipophilic, and other organic solvents, graphene oxide is dissolved in water or alcohol, and then the high-temperature alloy powder is added into the solution for dispersion, so that the full combination between the high-temperature alloy powder and graphene oxide nanosheets is facilitated.
(4) Because functional groups in the graphene oxide are easy to crack at high temperature, the graphene oxide can be reduced into graphene in a vacuum high-temperature environment, the graphene oxide/high-temperature alloy composite powder is filled into a stainless steel sheath for heating and degassing treatment, the graphene oxide/high-temperature alloy powder composite powder is prepared, and meanwhile, the sheath is sealed and welded, and the next step of powder thermal densification treatment can be directly carried out.
Drawings
FIG. 1 is a schematic view of a process flow for preparing graphene/superalloy powder composite powder;
FIG. 2 is a SEM surface morphology of the prepared graphene/superalloy powder composite powder;
fig. 3 is a microstructure morphology of the prepared graphene/superalloy composite powder after thermal densification molding.
Detailed Description
The technical solution of the present invention will be described clearly and completely with reference to fig. 1 to 3 and the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Firstly, adding 0.05-6 wt% of graphene oxide nanosheets into an alcohol solution, and carrying out ultrasonic stirring to uniformly disperse the graphene oxide in alcohol, wherein the ultrasonic stirring time is not less than 30 minutes. And standing the graphene oxide solution subjected to ultrasonic dispersion for 1-3 hours, and removing redundant alcohol.
Then adding the high-temperature alloy powder prepared by the AA method or the PREP method into the graphene oxide solution in batches. The high-temperature alloy powder added each time is 200-1000 g, the powder granularity is not more than-200 meshes, and the mixed powder is continuously mechanically stirred. The high-temperature alloy powder is observed to roll in the container fully in the stirring process, the deposition of the high-temperature alloy powder at the bottom of the container is avoided, and the graphene oxide is ensured to be uniformly dispersed in the high-temperature alloy powder. If the powder is agglomerated and the powder is difficult to stir due to bottom sinking in the stirring process, properly adding alcohol for dilution and then continuing stirring.
And finally, putting the prepared graphene oxide/high-temperature alloy powder into a drying furnace at the temperature of 50-100 ℃ for drying for 10-24 hours. Loading the dried graphene oxide/high-temperature alloy composite powder into a stainless steel sheath, performing vacuum degassing and heating treatment on the sheath,vacuum degree is less than or equal to 5 multiplied by 10-3Pa, and the temperature is 200-400 ℃ to obtain the graphene/high-temperature alloy composite powder.
Detailed description is shown in the schematic flow chart of the preparation process of the graphene/high-temperature alloy powder composite powder in figure 1.
The first embodiment is as follows:
and smelting the powder superalloy by adopting a ZG25 vacuum induction furnace to prepare an FGH96 powder superalloy master alloy ingot. Then preparing 20kg of high-temperature alloy powder by adopting an argon atomization method (AA method), and sieving the powder to obtain FGH96 high-temperature alloy powder with the granularity of-250 meshes. Preparing graphene oxide nano sheets by adopting a redox method, evenly dividing 1g of graphene oxide nano sheets into 2 parts by weight, respectively dissolving the graphene oxide nano sheets in 300ml of alcohol, and carrying out ultrasonic treatment on the graphene oxide solution by adopting a cell crusher, wherein the ultrasonic working time is 40 minutes. And standing the graphene oxide solution subjected to ultrasonic treatment for 2 hours, and removing the excessive alcohol on the upper part of the container. The prepared 2kg of FGH96 was evenly divided into 10 parts of powder, each of which was 200g, and the powder was added to the graphene oxide solution and continuously stirred with a mechanical stirrer. And fully stirring the graphene oxide/high-temperature alloy mixed powder for 1h, removing the graphene oxide/high-temperature alloy composite powder, and placing the graphene oxide/high-temperature alloy composite powder in a drying furnace for drying. The temperature of the drying furnace is adjusted to be 60 ℃, and the drying time is 16 h. And (3) putting the dried composite powder into a stainless steel sheath with the diameter of 80mm and the height of 110mm, and continuously vibrating to ensure the powder filling rate. After the composite powder is filled in the sheath, the sheath is vacuumized, gradually heated to 200 ℃, and vacuumized to 5 multiplied by 10-3Keeping the temperature for 12h after Pa, and sealing and welding the sheath to finish the preparation of the nickel-based high-temperature alkene alloy composite powder.
Example two:
and smelting the powder high-temperature alloy by adopting a ZG25 vacuum induction furnace to prepare a U720 high-temperature alloy master alloy ingot. Then preparing 10kg of high-temperature alloy powder by adopting an argon atomization method (AA method), and sieving the powder to obtain the U720 high-temperature alloy powder with the powder granularity of-300 meshes. Preparing graphene oxide nano-sheets by adopting a redox method, evenly dividing 360g graphene oxide nano-sheets into 6 parts by weight, respectively dissolving the graphene oxide nano-sheets in 300ml of alcohol, and oxidizing by adopting a cell crusherAnd carrying out ultrasonic treatment on the graphene solution, wherein the ultrasonic working time is 30 minutes. And standing the graphene oxide solution subjected to ultrasonic treatment for 2 hours, and removing the excessive alcohol on the upper part of the container. The prepared 6kg of U720 is evenly divided into 6 parts, each part is 1kg of powder, the powder is added into the graphene oxide solution, and a mechanical stirrer is adopted for continuous stirring. And fully stirring the graphene oxide/high-temperature alloy mixed powder for 1.5h, removing the graphene oxide/high-temperature alloy composite powder, and placing the graphene oxide/high-temperature alloy composite powder in a drying furnace for drying. The temperature of the drying furnace is adjusted to be 80 ℃, and the drying time is 10 h. And (3) putting the dried composite powder into a stainless steel sheath with the diameter of 120mm and the height of 128mm, and continuously vibrating to ensure the powder filling rate. After the composite powder is filled in the sheath, the sheath is vacuumized, gradually heated to 400 ℃, and vacuumized to 5 x 10- 3Keeping the temperature for 3h after Pa, and sealing and welding the sheath to finish the preparation of the nickel-based high-temperature alkene alloy composite powder.
The left and right graphs of fig. 2 and 3 show the test results of samples corresponding to examples 1 and 2, respectively.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.
Claims (2)
1. A preparation method of nickel-based high-temperature alkene alloy powder is characterized by comprising the following steps: the preparation method comprises the following steps: 1) dissolving graphene oxide nanosheets in water or alcohol, performing ultrasonic stirring dispersion, standing the graphene oxide solution, and removing excess water or alcohol above the graphene oxide solution; 2) adding a small amount of nickel-based superalloy powder prepared by an AA method or a PREP method into a graphene oxide solution in batches, and continuously mechanically stirring; 3) repeatedly washing the mixed powder, and drying the powder in an oven to obtain graphene oxide/high-temperature alloy composite powder; 4) then carrying out surface degassing treatment on the graphene oxide/high-temperature alloy powder, and filling the degassed mixed powder into a stainless steel sheath for sealing welding to prepare graphene/high-temperature alloy composite powder;
the graphene oxide nanosheet is prepared by adopting a redox method or a pyrolysis method, has a lamellar structure with a single layer or a plurality of atomic layer thicknesses, and is less than 10nm in thickness;
in the graphene oxide solution, the content of graphene oxide is 0.05 wt% -6 wt%; the ultrasonic stirring time is not less than 30 minutes, the stirring frequency is 2 seconds of ultrasound, and the gap is 5 seconds;
standing the graphene oxide solution for 1-3 h;
the granularity of the nickel-based superalloy powder is not more than-200 meshes;
the alloy powder is added in batches in a small amount, and the weight of the powder added in each batch is 200-1000 g;
the mechanical stirring time is not less than 40 minutes;
washing the composite powder for 3-5 times;
the vacuum degree of the degassing treatment is less than or equal to 5.0 multiplied by 10-3Pa, degassing temperature of 200-400 ℃ and degassing time of 3-12 h.
2. The method of preparing a nickel-base-superalloy powder of claim 1, comprising: the temperature of the oven is 50-100 ℃, and the drying time is 10-24 h.
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