CN110777277A - Graphene oxide aluminum-based composite material manufactured by laser deposition and preparation method thereof - Google Patents
Graphene oxide aluminum-based composite material manufactured by laser deposition and preparation method thereof Download PDFInfo
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Abstract
A graphene oxide aluminum-based composite material manufactured by laser deposition and a preparation method thereof belong to the field of metal-based composite materials. The preparation method of the graphene oxide aluminum-based composite material comprises the following steps: adding the graphene oxide solution, the aluminum-based powder, the ball milling balls and the solvent into a ball milling tank for wet ball milling to obtain graphene oxide aluminum-based composite powder; the graphene oxide aluminum-based composite material is used as a raw material, and is prepared by a Laser Deposition Manufacturing (LDM) method. According to the preparation method, the effect that graphene oxide is attached to the surface of the powder material is achieved through low-temperature wet ball milling by utilizing the synergistic effect of the alloy powder material and the ball milling balls, the graphene oxide is uniformly and effectively dispersed in the aluminum matrix, the graphene oxide is ensured not to react with the aluminum matrix, the feasibility of laser deposition manufacturing of the graphene oxide aluminum matrix composite material is realized, and the mechanical property of the graphene oxide aluminum matrix composite material is enhanced.
Description
Technical Field
The invention relates to the technical field of metal matrix composite materials, in particular to a graphene oxide aluminum matrix composite material manufactured by laser deposition and a preparation method thereof.
Background
Laser Additive Manufacturing (LAM) is an additive manufacturing technique using laser as an energy source, has the advantage of high energy density, and can be used for machining and manufacturing of difficult-to-machine metal, complex-structure and thin-walled parts. The Laser additive Manufacturing is divided into Selective Laser Melting (SLM) and Laser Deposition Manufacturing (LDM) based on different forming principles, wherein the SLM is a process of spreading powder bed, completely melting the spread metal powder by Laser according to a predetermined scanning path, and performing solidification molding. The LDM is used for synchronously feeding powder, and melting, rapidly solidifying and depositing the synchronously fed metal powder layer by adopting laser according to a preset processing path. The LDM method does not need a mould, the near-net-shape manufacturing of the fully-compact and high-performance metal structural part is completed by the CAD model of the part in one step, the large-size part can be manufactured, and the research is wider.
In the prior art, laser additive manufacturing aluminum alloy is mainly formed by SLM, LDM research is less, because for materials manufactured by laser additive manufacturing, metal powder is generally used, the quality of the metal powder has great influence on the quality of finally formed materials, for light alloy powder, powder feeding of LDM technology is difficult, the aluminum alloy has strong reflectivity to laser, a laser with higher power is required, the aluminum alloy is easy to oxidize to form an oxide film in the forming process, so that a spheroidizing effect is formed in a molten pool, and pores appear in the aluminum alloy.
The graphene has the advantages of large specific surface area, high strength, high toughness, good heat and electricity conductivity, low thermal expansion coefficient and the like. The aluminum-based composite material is one of the most common and important materials in the metal-based composite material, and has the advantages of light weight, low density, good damping performance, corrosion resistance, good heat conductivity, low thermal expansion coefficient and the like. The method has wide application in the fields of aerospace, automobiles and the like. However, the aluminum material has low hardness, is easy to crack, and affects safety, and the prior art can modify the surface of the aluminum material so as to improve the performance of the aluminum material. However, the requirements of the development of the existing scientific and technological life, the automobile field and the aerospace field on the material performance are higher and higher, and the traditional ceramic fiber and particle reinforcement cannot meet the requirements of the material in a special environment. The graphene reinforced aluminum-based composite material is necessary to be prepared by virtue of the excellent performance of graphene, and the graphene aluminum-based composite material has a good application prospect in the field of future materials. However, graphene and a metal matrix have the problems of poor wettability, easy interface reaction, easy aggregation of graphene, poor dispersibility in the matrix and the like.
In the prior patent publications, the key problem of preparing graphene aluminum matrix composite materials is to uniformly and effectively disperse graphene in an aluminum matrix and reduce the interface reaction between graphene and the aluminum matrix.
Disclosure of Invention
The invention aims to overcome the defects of difficult laser additive forming of aluminum alloy, easy agglomeration of graphene in an aluminum matrix and poor wettability between the graphene and the aluminum matrix in the prior art, and provides a graphene oxide aluminum matrix composite material prepared by laser deposition and a preparation method thereof. According to the preparation method, the effect that graphene oxide is attached to the surface of the powder material is achieved through low-temperature wet ball milling by utilizing the synergistic effect of the alloy powder material and the ball milling balls, so that the graphene oxide is uniformly and effectively dispersed in the aluminum matrix, and the graphene oxide is prevented from reacting with the aluminum matrix, so that the graphene oxide aluminum-based composite powder material is obtained. And then obtaining the graphene oxide aluminum-based composite material in a forming mode of laser deposition manufacturing.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method for manufacturing a graphene oxide aluminum-based composite material by laser deposition comprises the following steps:
step 1: stock preparation
Adding graphene oxide into a solvent, and performing ultrasonic oscillation for 1-3 hours to obtain a graphene oxide solution; wherein, according to the solid-liquid ratio, the graphene oxide: solvent ═ (0.05-0.1) g: (120-200) mL;
step 2: preparation of graphene oxide aluminum-based composite powder by low-temperature wet ball milling
(1) Adding an aluminum-based powder material, a graphene oxide solution, ball milling balls and a solvent into a cleaned ball milling tank according to a ratio, vacuumizing, and performing ball milling at a temperature of 20-200 ℃ to obtain a ball milling product; the ball material ratio is (3-6) according to the mass ratio: 1; according to the volume ratio, (ball milling ball + aluminum base powder): solvent ═ (1-3): 1; according to the mass ratio, the graphene oxide: (aluminum powder + graphene oxide) ═ 0.05 to 0.1: 100, respectively;
wherein the particle size of the aluminum-based powder is 60-180 meshes; the grain diameter of the ball grinding ball is 2-8 mm;
the ball milling parameters are as follows: the ball milling speed is 200-500r/min, the ball milling adopts interval ball milling, the total ball milling time is 8-20h, and the ball milling is stopped for 5-15min every 30 min;
(2) taking out the ball-milled product, airing, and separating the obtained powder from the ball-milled balls to obtain graphene oxide aluminum-based composite powder;
and step 3: preparation of graphene oxide aluminum-based composite material by laser deposition
Preparing a graphene oxide aluminum-based composite material by using a Laser Deposition Manufacturing (LDM) method by using a graphene oxide aluminum-based composite powder as a raw material; the Laser Deposition Manufacturing (LDM) method comprises the following processes: argon is used as protective gas, the diameter of a light spot is 3-5mm, the laser power is 1.6KW-2.2KW, the scanning speed is 3mm/s-7mm/s, the powder feeding speed is 0.8-1.6r/s, the scanning interval is 1-3mm, and the scanning layer thickness is 0.5-1 mm.
In the step 1, the solvent is absolute ethyl alcohol or acetone.
In the step 1, the ultrasonic frequency of the ultrasonic oscillation is preferably 40 KHz.
In the step 1, the temperature of ultrasonic oscillation is below 40 ℃.
In the step 2(1), the aluminum-based powder material is preferably a cast Si-Al-Mg-based aluminum alloy base material or a cast Si-Al-based aluminum alloy base material, specifically one of AlSi10Mg, ZL114A, ZL101A, 6061, and AlSi 12.
In the step 2(1), the ball grinding ball is one of a stainless steel ball, a zirconia ball or an agate ball, and is placed in absolute ethyl alcohol for ultrasonic oscillation for 20-40min before use.
In the step 2(1), the solvent is absolute ethyl alcohol or acetone.
In the step 2(1), the vacuum degree is 2.5X 10
-2Pa-4.0×10
-2Pa。
In the step 2(2), the sphericity of the prepared graphene oxide aluminum-based composite powder is 0.75-9.9.
In the step 3, the laser power is preferably 1.8KW-2.0KW, more preferably 1.8KW, and the scanning speed is preferably 3mm/s-5mm/s, more preferably 5 mm/s.
The graphene oxide aluminum-based composite material prepared by laser deposition is prepared by the preparation method.
Compared with an aluminum-based base material, the tensile strength of the prepared graphene oxide aluminum-based composite material prepared by laser deposition is improved by 20-55%, and the elongation is improved by 100-120%.
The invention relates to a graphene oxide aluminum-based composite material prepared by laser deposition and a preparation method thereof, and the graphene oxide aluminum-based composite material has the beneficial effects that:
1. the graphene oxide aluminum-based composite powder is prepared by a two-step method of ultrasonic oscillation dispersion and vacuum low-temperature wet ball milling; the first step is as follows: adding graphene into a solvent, carrying out ultrasonic oscillation at a low temperature (below 40 ℃), and carrying out a second step: and (5) carrying out low-temperature vacuum wet ball milling. The problem of agglomeration of graphene in a matrix can be effectively solved by using a two-step method of absolute ethyl alcohol solution dispersion and wet ball milling, and the interface reaction between the graphene and the matrix can be effectively avoided by adding a solvent and reducing the temperature. The graphene can be uniformly dispersed in the matrix, and meanwhile, the graphene mixed in the aluminum-based powder is uniformly attached to the surface of the aluminum-based powder.
2. According to the invention, the laser absorption of the aluminum alloy can be improved by controlling the laser deposition manufacturing technology, the feasibility of processing the graphene aluminum-based composite material by the laser deposition manufacturing technology is verified, and the performance of the prepared graphene oxide aluminum-based composite material workpiece is enhanced.
Drawings
FIG. 1 is a flow chart of a preparation process of the preparation method of the graphene oxide aluminum-based composite material by laser deposition;
FIG. 2 is an SEM image of 350 times scanning electron microscope of aluminum-based powder particles in example 2 of the present invention;
FIG. 3 is an SEM image of the aluminum-based powder of example 2 under a scanning electron microscope of 1K times;
fig. 4 is an SEM image of 600 times scanning electron microscope of the graphene oxide aluminum-based composite powder prepared in example 2 of the present invention;
fig. 5 is an SEM image of graphene oxide coated on the surface of the graphene oxide aluminum-based composite powder prepared in embodiment 2 of the present invention under a scanning electron microscope of 10K times;
fig. 6 is an SEM image of graphene oxide coated on the surface of the graphene oxide aluminum-based composite powder prepared in embodiment 2 of the present invention under a scanning electron microscope of 20K times;
FIG. 7 is a comparison graph of room temperature mechanical properties of graphene oxide aluminum-based composite manufactured by laser deposition;
fig. 8 is a fracture morphology diagram of the graphene oxide aluminum-based composite material prepared in embodiment 2 under a scanning electron microscope of 1K times;
fig. 9 is a fracture morphology diagram of the graphene oxide aluminum-based composite material prepared in embodiment 2 under a scanning electron microscope of 5K times;
fig. 10 is a fracture morphology diagram of the graphene oxide aluminum-based composite material prepared in embodiment 4 of the present invention under a scanning electron microscope of 1K times;
fig. 11 is a fracture morphology diagram of the graphene oxide aluminum-based composite material prepared in embodiment 4 of the present invention under a scanning electron microscope of 5K times;
FIG. 12 is a fracture morphology of pure ZL114A of comparative example 1 under a scanning electron microscope of 438 times;
FIG. 13 is a fracture morphology of pure ZL114A of comparative example 1 of the present invention under a scanning electron microscope of 10K times.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, reagents and equipment used are commercially available or known in the art unless otherwise specified.
In the following examples, the preparation method of the graphene oxide used was: uniformly mixing 23mL of concentrated sulfuric acid, 4g of potassium permanganate and 1g of graphite powder, reacting at 40 ℃ for 30min, diluting with deionized water, adding 5mL of 30% hydrogen peroxide with mass concentration to remove the potassium permanganate, washing with 250mL of 10% dilute hydrochloric acid with mass concentration, and finally drying by blowing at the temperature of not higher than 30 ℃ to obtain the graphene oxide.
Example 1
A preparation method for manufacturing a graphene oxide aluminum-based composite material by laser deposition is disclosed, wherein a process flow schematic diagram is shown in figure 1, and comprises the following steps:
step 1: stock preparation
(1) Before ball milling, an aluminum-based powder (60-180 meshes), prepared graphene oxide and a 2-8mm ball milling ball are required to be prepared, wherein the ball milling ball is one of a stainless steel ball, a zirconia ball and an agate ball, the embodiment adopts the stainless steel ball and a solvent (such as absolute ethyl alcohol and acetone, and the embodiment adopts the absolute ethyl alcohol);
(2) adding 0.1g of graphene oxide into 120mL of absolute ethyl alcohol before use, carrying out ultrasonic oscillation for 2h at 40KHz, and controlling the ultrasonic oscillation temperature to be below 40 ℃ to obtain a graphene oxide solution;
(3) adding stainless steel ball into anhydrous alcohol before use, and performing ultrasonic oscillation for 20-40 min;
step 2: preparation of graphene oxide aluminum-based composite powder by low-temperature wet ball milling
Adding an aluminum-based powder material AlSi10Mg, a graphene oxide solution, a stainless steel ball and absolute ethyl alcohol into a ball milling tank cleaned by alcohol in sequence; the ball milling tank is vacuumized to 4.0 multiplied by 10 by a vacuum pump
-2Pa; wherein, the ball material ratio is 5: 1, the volume ratio of the stainless steel ball (comprising an aluminum-based powder material AlSi10Mg) to the absolute ethyl alcohol is (the stainless steel ball + the aluminum-based powder material): absolute ethanol ═ 2: 1; the ball milling speed is 300r/min, the ball milling time is 10 hours, and the ball milling is stopped for 10min every 30 min;
taking out and airing the powder after the ball milling is stopped; separating the powder from the stainless steel ball by using a sieve to obtain graphene oxide aluminum-based composite powder;
and step 3: preparation of graphene oxide aluminum-based composite material by laser deposition
The graphene oxide aluminum-based composite material is prepared by a Laser Deposition Manufacturing (LDM) technology, and the process parameters are as follows: argon is used as protective gas, the diameter of a light spot is 4mm, the laser power is 1.8KW, the scanning speed is 5mm/s, the powder feeding speed is 0.8r/s, the scanning interval is 2mm, and the thickness of the scanning layer is 0.6 mm.
Example 2
A preparation method for manufacturing a graphene oxide aluminum-based composite material by laser deposition comprises the following steps:
step 1: stock preparation
(1) All that is required to prepare prior to ball milling is: the aluminum-based powder material ZL114A (60-180 mesh), the prepared graphene oxide and the 2-8mm ball grinding ball are one of stainless steel balls, zirconia balls and agate balls, in this embodiment, zirconia balls and a solvent (such as absolute ethyl alcohol and acetone, in this embodiment, absolute ethyl alcohol) are adopted;
scanning the aluminum-based powder ZL114A in this example, SEM images of the powder under different magnifications are shown in fig. 2 and fig. 3, and it can be seen from the images that the powder shows the overall morphology under low-power SEM, the surface is smooth, the powder has better sphericity, and is suitable for powder feeding printing, and after the magnification, it is seen that the crystal grains have no obvious difference from the low-power morphology.
(2) Adding 0.1g of graphene oxide into 120mL of absolute ethyl alcohol before use, carrying out ultrasonic oscillation for 2h at 40KHz, and controlling the ultrasonic oscillation temperature to be below 40 ℃ to obtain a graphene oxide solution;
(3) adding zirconia balls into absolute ethyl alcohol before use, and carrying out ultrasonic oscillation for 30 min;
step 2: preparation of graphene oxide aluminum-based composite powder by low-temperature wet ball milling
According to the mass ratio, zirconia balls with the diameter of 2-8 mm: (cast aluminum powder ZL114A + graphene oxide) ═ 5: 1, cast aluminum powder ZL 114A: putting the graphene oxide, cast aluminum powder ZL114A and zirconia balls with the diameter of 2-8mm into a ball milling tank to form a mixture, and adding absolute ethyl alcohol into the ball milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 600: 120 in g: mL. The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10
-2And Pa, putting the ball milling tank into a ball mill, performing ball milling for 8 hours (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 250r/min, drying after ball milling, and separating the powder and the balls by using a sieve to obtain the graphene oxide aluminum-based composite powder.
Scanning the graphene oxide aluminum-based composite powder prepared in the embodiment, wherein SEM images of the graphene oxide aluminum-based composite powder prepared in the embodiment under different magnifications are shown in fig. 4, fig. 5 and fig. 6, and from the above figures, it can be seen that the graphene oxide powder uniformly covers the surface of the cast aluminum powder ZL114A, the surface of the prepared graphene oxide aluminum-based composite powder is rough, but has a better sphericity suitable for powder feeding printing, and graphene sheets can be clearly seen to be attached to the surface of the powder under high magnifications.
The sphericity of the prepared graphene oxide aluminum-based composite powder is 0.75-9.9.
And step 3: preparation of graphene oxide aluminum-based composite material by laser deposition
And (2) carrying out forming processing of a laser deposition manufacturing technology on the graphene oxide aluminum-based composite powder, wherein argon is used as protective gas, the diameter of a light spot is 4mm, the laser power is 2KW, the powder feeding speed is 0.8r/s at the scanning speed of 5mm/s, the scanning distance is 2mm, and the scanning layer thickness is 0.6mm, so as to obtain the graphene oxide aluminum-based composite material.
According to GB/T228.1-2010GB metal material room temperature tensile test standard, a tensile plate is taken to perform room temperature mechanical property detection experiments, the tensile strength and the elongation at break are tested, and the results are shown in Table 1.
At a mass fraction of 0.1% of graphene oxide, the fracture morphology of the graphene oxide aluminum-based composite material is shown in fig. 8 and 9, a large number of elongated reticular shearing pits exist on the fracture surface, and the pits are elongated, have larger sizes and are more inclined and deeper, and show that the fracture property is ductile fracture. This fracture phenomenon indicates that the material has better toughness.
Example 3
A preparation method for manufacturing a graphene oxide aluminum-based composite material by laser deposition comprises the following steps:
step 1: stock preparation
(1) Before ball milling, an aluminum-based powder (60-180 meshes), prepared graphene oxide and 2-8mm ball milling balls are required to be prepared, wherein the ball milling balls are one of stainless steel balls, zirconia balls and agate balls, agate balls and solvents (such as absolute ethyl alcohol and acetone, and absolute ethyl alcohol is adopted in the embodiment);
(2) adding 0.1g of graphene oxide into 120mL of absolute ethyl alcohol before use, carrying out ultrasonic oscillation for 2h at 40KHz, and controlling the ultrasonic oscillation temperature to be below 40 ℃ to obtain a graphene oxide solution;
(3) adding the agate balls into absolute ethyl alcohol before use, and carrying out ultrasonic oscillation for 30 min;
step 2: preparation of graphene oxide aluminum-based composite powder by low-temperature wet ball milling
2-8mm agate balls in mass ratio: (cast aluminum powder ZL114A + graphene oxide) ═ 5: 1, cast aluminum powder ZL 114A: putting the graphene oxide, cast aluminum powder ZL114A and 2-8mm agate balls into a ball milling tank to form a mixture, and adding absolute ethyl alcohol into the ball milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 600: 120 in g: mL. The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10
-2And Pa, putting the ball milling tank into a ball mill, performing ball milling for 8 hours (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 250r/min, drying after ball milling, and separating the powder and the balls by using a sieve to obtain the graphene oxide aluminum-based composite powder.
And step 3: preparation of graphene oxide aluminum-based composite material by laser deposition
And (2) carrying out forming processing of a laser deposition manufacturing technology on the graphene oxide aluminum-based composite powder, wherein argon is used as protective gas, the diameter of a light spot is 3mm, the laser power is 1.8KW, the scanning speed is 5mm/s, the powder feeding speed is 0.8r/s, the scanning interval is 2mm, and the scanning layer thickness is 0.6mm, so as to obtain the graphene oxide aluminum-based composite material.
According to GB/T228.1-2010GB metal material room temperature tensile test standard, a tensile plate is taken to perform room temperature mechanical property detection experiments, the tensile strength and the elongation at break are tested, and the results are shown in Table 1.
Example 4
A preparation method for manufacturing a graphene oxide aluminum-based composite material by laser deposition comprises the following steps:
step 1: stock preparation
(1) Before ball milling, an aluminum-based powder (60-180 meshes), prepared graphene oxide and a 2-8mm ball milling ball are required to be prepared, wherein the ball milling ball is one of a stainless steel ball, a zirconia ball and an agate ball, the embodiment adopts the stainless steel ball and a solvent (such as absolute ethyl alcohol and acetone, and the embodiment adopts the absolute ethyl alcohol);
(2) adding 0.1g of graphene oxide into 120mL of absolute ethyl alcohol before use, carrying out ultrasonic oscillation for 2h at 40KHz, and controlling the ultrasonic oscillation temperature to be below 40 ℃ to obtain a graphene oxide solution;
(3) adding the stainless steel ball into absolute ethyl alcohol before use, and carrying out ultrasonic oscillation for 30 min;
step 2: preparation of graphene oxide aluminum-based composite powder by low-temperature wet ball milling
According to the mass ratio, stainless steel balls with the diameter of 2-8 mm: (cast aluminum powder ZL114A + graphene oxide) ═ 5: 1, cast aluminum powder ZL 114A: and (2) placing the graphene oxide, cast aluminum powder ZL114A and a stainless steel ball with the diameter of 2-8mm into a ball milling tank to form a mixture, and adding absolute ethyl alcohol into the ball milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 600: 120 in g: mL. The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10
-2And Pa, putting the ball milling tank into a ball mill, performing ball milling for 8 hours (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 250r/min, drying after ball milling, and separating the powder and the balls by using a sieve to obtain the graphene oxide aluminum-based composite powder.
And step 3: preparation of graphene oxide aluminum-based composite material by laser deposition
And (2) carrying out forming processing of a laser deposition manufacturing technology on the graphene oxide aluminum-based composite powder, wherein argon is used as protective gas, the diameter of a light spot is 5mm, the laser power is 2KW, the scanning speed is 5mm/s, the powder feeding speed is 0.8r/s, the scanning interval is 2mm, and the scanning layer thickness is 0.6mm, so as to obtain the graphene oxide aluminum-based composite material.
According to GB/T228.1-2010GB metal material room temperature tensile test standard, a tensile plate is taken to perform room temperature mechanical property detection experiments, the tensile strength and the elongation at break are tested, and the results are shown in Table 1.
When the mass fraction of the graphene oxide is 0.05%, the fracture morphology of the graphene oxide aluminum-based composite material is shown in fig. 10 and fig. 11, and a large number of equiaxed pits exist on the fracture surface and are elongated along the loading direction, which indicates that the fracture property is ductile fracture, and the material has better toughness.
Example 5
A preparation method for manufacturing a graphene oxide aluminum-based composite material by laser deposition comprises the following steps:
step 1: stock preparation
(1) Before ball milling, an aluminum-based powder (60-180 meshes), prepared graphene oxide and a 2-8mm ball milling ball are required to be prepared, wherein the ball milling ball is one of a stainless steel ball, a zirconia ball and an agate ball, in the embodiment, the zirconia ball and a solvent (such as absolute ethyl alcohol and acetone, and in the embodiment, the absolute ethyl alcohol is adopted);
(2) adding 0.1g of graphene oxide into 120mL of absolute ethyl alcohol before use, carrying out ultrasonic oscillation for 2h at 40KHz, and controlling the ultrasonic oscillation temperature to be below 40 ℃ to obtain a graphene oxide solution;
(3) adding zirconia balls into absolute ethyl alcohol before use, and carrying out ultrasonic oscillation for 30 min;
step 2: preparation of graphene oxide aluminum-based composite powder by low-temperature wet ball milling
According to the mass ratio, zirconia balls with the diameter of 2-8 mm: (cast aluminum powder ZL114A + graphene oxide) ═ 5: 1, cast aluminum powder ZL 114A: placing the graphene oxide, cast aluminum powder ZL114A and zirconia balls with the diameter of 2-8mm into a ball milling tank to form a mixture, adding absolute ethyl alcohol into the ball milling tank, and mixing the mixture and the absolute ethyl alcoholThe proportion of the water ethanol is 600: 120 in g: mL. The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10
-2And Pa, putting the ball milling tank into a ball mill, performing ball milling for 8 hours (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 250r/min, drying after ball milling, and separating the powder and the balls by using a sieve to obtain the graphene oxide aluminum-based composite powder.
And step 3: preparation of graphene oxide aluminum-based composite material by laser deposition
And (2) carrying out forming processing of a laser melting deposition manufacturing technology on the graphene oxide aluminum-based composite powder, wherein argon is used as protective gas, the diameter of a light spot is 3mm, the laser power is 1.8KW, the scanning speed is 5mm/s, the powder feeding speed is 0.8r/s, the scanning interval is 2mm, and the scanning layer thickness is 0.6mm, so as to obtain the graphene oxide aluminum-based composite material.
Example 6
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 1.6KW, and the scanning speed is 3 mm/s.
The other ways are the same.
Example 7
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 1.8KW, and the scanning speed is 3 mm/s.
The other ways are the same.
Example 8
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 2KW, the scanning speed is 3mm/s, the powder feeding speed is 1.4r/s, the scanning interval is 2mm, and the scanning layer thickness is 0.8 mm.
The other ways are the same.
Example 9
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 2.2KW, and the scanning speed is 3 mm/s.
The other ways are the same.
Example 10
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 1.6KW, and the scanning speed is 5 mm/s.
The other ways are the same.
Example 11
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 2.2KW, and the scanning speed is 5 mm/s.
The other ways are the same.
Example 12
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 1.6KW, the scanning speed is 7mm/s, the powder feeding speed is 1.6r/s, the scanning interval is 1mm, and the scanning layer thickness is 0.5 mm.
The other ways are the same.
Example 13
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 1.8KW, and the scanning speed is 7 mm/s.
The other ways are the same.
Example 14
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 2.0KW, and the scanning speed is 7 mm/s.
The other ways are the same.
Example 15
A preparation method of a graphene oxide aluminum-based composite material manufactured by laser deposition, which is the same as that in example 1, except that:
in step 3, the laser power is 2.2KW, the scanning speed is 7mm/s, the powder feeding speed is 1.2r/s, the scanning distance is 3mm, and the scanning layer thickness is 1 mm.
The other ways are the same.
Comparative example 1
The ZL114A powder material is subjected to forming processing of a laser deposition manufacturing technology, argon is used as protective gas, the laser power is 2KW, the scanning speed is 5mm/s, the powder feeding speed is 0.8r/s, the scanning distance is 2mm, and the scanning layer thickness is 0.6 mm. .
According to GB/T228.1-2010GB metal material room temperature tensile test standard, a tensile plate is taken to perform room temperature mechanical property detection experiments, the tensile strength and the elongation at break are tested, and the results are shown in Table 1.
SEM images of the fracture morphology of pure ZL114A are shown in fig. 12 and 13, without obvious macroscopic plastic deformation features, and the flush and bright fracture morphology indicates that the fracture property is brittle fracture, reflecting that pure ZL114A has lower ductility and poorer toughness.
TABLE 1 mechanical Properties of the tensile sheet of the examples
| Graphene oxide content (%) | Tensile strength (MPa) | Elongation (%) | |
| Example 2 | 0.1 | 230.1 | 6.39 |
| Example 4 | 0.05 | 205.4 | 6.12 |
| Comparative example 1 | 0 | 149.7 | 2.93 |
And the stress-strain curves of example 2, example 4 and comparative example 1 are shown in fig. 7, and it can be seen from fig. 7 that the tensile strength of the pure ZL114A material produced by laser deposition is the lowest, 149.7MPa, and the elongation is 2.93%. When the mass fraction of the graphene oxide is 0.05%, the tensile strength of the graphene oxide aluminum-based composite material manufactured by laser deposition is 205.4MPa, the elongation is 6.12%, and compared with pure ZL114A without the addition of the graphene oxide, the tensile strength is improved by 37.2%, and the elongation is improved by 108%. When the mass fraction of the graphene oxide is 0.1%, the tensile strength of the graphene oxide aluminum-based composite material manufactured by laser deposition is 230.1MPa, the elongation is 6.39%, and compared with pure ZL114A without the addition of the graphene oxide, the tensile strength is improved by 53.7%, and the elongation is improved by 118%. As can be seen from the results in table 1, the strength and elongation of the graphene oxide aluminum-based composite material gradually increase with the increase of the content of graphene oxide. The addition of the nano graphene oxide and the uniform dispersion of the nano graphene oxide in the aluminum matrix prevent the growth and coarsening of crystal grains in the processing process, and play a role in refining the crystal grains. The nano graphene oxide blocks the dislocation migration in the plastic deformation process of the graphene oxide aluminum-based composite material, provides the dislocation resistance, and simultaneously bears and transfers a part of load. The refinement of crystal grains, the obstruction of dislocation and the bearing and transmission of load play a role in improving the strength and the elongation of the graphene oxide aluminum-based composite material.
Claims (10)
1. A preparation method for manufacturing a graphene oxide aluminum-based composite material by laser deposition is characterized by comprising the following steps:
step 1: stock preparation
Adding graphene oxide into a solvent, and performing ultrasonic oscillation for 1-3 hours to obtain a graphene oxide solution; wherein, according to the solid-liquid ratio, the graphene oxide: solvent ═ (0.05-0.1) g: (120-200) mL;
step 2: preparation of graphene oxide aluminum-based composite powder by low-temperature wet ball milling
(1) Adding an aluminum-based powder material, a graphene oxide solution, ball milling balls and a solvent into a cleaned ball milling tank according to a ratio, vacuumizing, and performing ball milling at a temperature of 20-200 ℃ to obtain a ball milling product; the ball material ratio is (3-6) according to the mass ratio: 1; according to the volume ratio, (ball milling ball + aluminum base powder): solvent ═ (1-3): 1; according to the mass ratio, the graphene oxide: (aluminum powder + graphene oxide) ═ 0.05 to 0.1: 100, respectively;
wherein the particle size of the aluminum-based powder is 60-180 meshes; the grain diameter of the ball grinding ball is 2-8 mm;
the ball milling parameters are as follows: the ball milling speed is 200-500r/min, the ball milling adopts interval ball milling, the total ball milling time is 8-20h, and the ball milling is stopped for 5-15min every 30 min;
(2) taking out the ball-milled product, airing, and separating the obtained powder from the ball-milled balls to obtain graphene oxide aluminum-based composite powder;
and step 3: preparation of graphene oxide aluminum-based composite material by laser deposition
Preparing a graphene oxide aluminum-based composite material by using a laser deposition manufacturing method by using a graphene oxide aluminum-based composite powder as a raw material; the laser deposition manufacturing method comprises the following processes: argon is used as protective gas, the diameter of a light spot is 3-5mm, the laser power is 1.6KW-2.2KW, the scanning speed is 3mm/s-7mm/s, the powder feeding speed is 0.8-1.6r/s, the scanning interval is 1-3mm, and the scanning layer thickness is 0.5-1 mm.
2. The method for preparing graphene oxide aluminum-based composite material by laser deposition according to claim 1, wherein in the step 1, the solvent is absolute ethyl alcohol or acetone.
3. The method for preparing graphene oxide aluminum-based composite material by laser deposition according to claim 1, wherein in the step 2(1), the aluminum-based powder material is a cast Si-Al-Mg-based aluminum alloy base material or a cast Si-Al-based aluminum alloy base material, specifically one of AlSi10Mg, ZL114A, ZL101A, 6061 and AlSi 12.
4. The method for preparing the graphene oxide aluminum-based composite material by laser deposition according to claim 1, wherein in the step 2(1), the ball milling ball is one of a stainless steel ball, a zirconia ball or an agate ball, and is placed in absolute ethyl alcohol for ultrasonic oscillation for 20-40min before use.
5. The method for preparing graphene oxide aluminum-based composite material by laser deposition according to claim 1, wherein in the step 2(1), the solvent is absolute ethyl alcohol or acetone.
6. The method for preparing graphene oxide aluminum-based composite material by laser deposition according to claim 1, wherein in the step 2(1), the degree of vacuum is 2.5 x 10
-2Pa-4.0×10
-2Pa。
7. The method for preparing graphene oxide aluminum-based composite material by laser deposition according to claim 1, wherein in the step 2(2), the prepared graphene oxide aluminum-based composite powder has a sphericity of 0.75-9.9.
8. The method for preparing the graphene oxide aluminum-based composite material by laser deposition according to claim 1, wherein in the step 3, the laser power is 1.8KW-2.0KW, and the scanning speed is 3mm/s-5 mm/s.
9. The graphene oxide aluminum-based composite material prepared by laser deposition is characterized by being prepared by the preparation method of any one of claims 1-8.
10. The laser deposition method for preparing graphene oxide aluminum-based composite material according to claim 9, wherein the prepared graphene oxide aluminum-based composite material prepared by laser deposition has tensile strength improved by 20-55% and elongation improved by 100-120% compared with aluminum-based base material.
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