CN113172219A - Preparation method and application of graphene-reinforced AlSi10Mg nanocomposite - Google Patents
Preparation method and application of graphene-reinforced AlSi10Mg nanocomposite Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 73
- 239000000843 powder Substances 0.000 claims abstract description 71
- 239000008367 deionised water Substances 0.000 claims abstract description 48
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 48
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 30
- 239000000725 suspension Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 16
- 230000010355 oscillation Effects 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 238000007639 printing Methods 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 abstract description 15
- 239000000203 mixture Substances 0.000 abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 6
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Abstract
The invention discloses a preparation method and application of a graphene-reinforced AlSi10Mg nano composite material, which comprises the steps of mixing graphene oxide with deionized water to form a suspension, mixing the suspension at the high temperature of 800 ℃ and in the atmosphere of ammonia gas, dissolving ammonia gas into deionized water to be alkaline, decomposing the ammonia gas into nitrogen gas and hydrogen gas at the high temperature, using the nitrogen gas as a protective gas and the hydrogen gas as a reducing atmosphere, accelerating the reduction of the graphene oxide in the alkaline and high-temperature environment, enabling the reduced graphene to be more uniformly distributed in an AlSi10Mg matrix in the high-temperature environment, synchronously realizing the reducing atmosphere and the protective atmosphere by utilizing the decomposition of the ammonia gas in the high-temperature environment, ensuring uniform proportion, leading the prepared graphene-reinforced AlSi10Mg nano composite material to be completely reduced and the graphene to be more uniformly distributed, and avoiding the agglomeration of the graphene by utilizing the deionized water to firstly mix, the interface bonding degree and wettability of the reinforcing phase and the matrix are higher, and the powder flowability is better.
Description
Technical Field
The invention relates to the field of AlSi10Mg nano composite materials and metal additive manufacturing, in particular to a preparation method and application of a graphene reinforced AlSi10Mg nano composite material.
Background
The 3D printing technology is a technology that realizes manufacturing by gradual accumulation of materials based on a stacking principle. The method comprises the steps of cutting a 3D model of a formed part into a series of thin slices with certain thickness by using a computer, manufacturing each layer of thin slice from top to bottom by using 3D printing equipment, and forming a three-dimensional solid part in an overlapping mode. The technology can realize the manufacture of complex structures which can not be processed by the traditional process without the traditional cutter. The 3D printing technology has the advantages of no limitation of part structures and materials, short period, simple production process and the like, and is a high and new manufacturing technology with infinite prospect.
The metal additive manufacturing technology has ultrahigh freedom degree in manufacturing, and can realize precise integrated forming of any structural member with a complex appearance. The development is very rapid in recent years, and the method becomes the most representative technology in the additive manufacturing. At present, the technology has great potential in the fields of medical treatment, aerospace and the like, and the technology overturns the traditional processing technology in the specific application field. The selective laser melting technology, the electron beam melting forming technology and the laser metal deposition technology in the metal additive manufacturing technology all need metal powder as raw materials. Therefore, the preparation of the metal powder material with excellent performance plays a crucial role in developing metal additive manufacturing technology.
There are many metal powders that have been used in the field of metal additive manufacturing, such as aluminum alloy powder, titanium alloy powder, nickel-based superalloy powder, and stainless steel powder. Each type of metal powder has a number of series brand classes. Different metal powders have their own advantages and disadvantages and can be used in specific applications. The aluminum alloy has low density, excellent mechanical properties and multiple characteristics, is an indispensable lightweight structural material and functional material in the high-tech fields of military national defense, aerospace and the like, and has wide application prospect and research value in the fields of aerospace, transportation and the like. The SLM technology is applied to form single-piece or small-batch aluminum alloy parts, so that the material utilization rate can be greatly improved, the manufacturing period is shortened, and the manufacturing cost is reduced. However, with the development of science and technology, the conventional alloy or simple substance material has been unable to meet the mechanical properties of the parts. Therefore, it is one of the hot issues of people in the present stage to research a more excellent powder preparation method.
Disclosure of Invention
The invention aims to provide a preparation method and application of a graphene-reinforced AlSi10Mg nanocomposite, so as to overcome the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a graphene reinforced AlSi10Mg nanocomposite comprises the following steps:
s1, uniformly mixing graphene oxide powder and deionized water to obtain a suspension A, wherein the mass ratio of the graphene oxide powder to the volume ratio of the deionized water is (1-20 mg): 1 ml;
s2, uniformly mixing the suspension A and the AlSi10Mg powder in an ammonia atmosphere at the mixing temperature of 500-800 ℃, and drying in a vacuum environment to obtain the graphene reinforced AlSi10Mg nanocomposite.
Furthermore, the number of the thin film layers of the graphene oxide powder is 1-2.
Furthermore, the particle size of the graphene oxide powder is 0.2-5nm, and the purity is 99.9%.
Further, uniformly mixing the graphene oxide powder and deionized water by adopting an ultrasonic oscillation method to obtain a graphene oxide-deionized water turbid liquid.
Further, the particle size of the AlSi10Mg powder is micron-sized or nano-sized.
Furthermore, the mass of the graphene oxide in the suspension A is 0.3-0.9% of the mass of the AlSi10Mg powder.
Further, in step S2, first, a predetermined amount of graphene oxide-deionized water suspension and AlSi10Mg powder are loaded into a homogenizer, and then ammonia gas is introduced, and the flow rate of ammonia gas is kept at 100-.
Further, the temperature of vacuum drying is 110 ℃, and the time is not less than 12 h.
A printing and forming method of composite materials adopts a selective laser melting technology or an electron beam melting technology to print and form the composite materials obtained by the method.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a preparation method of a graphene-reinforced AlSi10Mg nano composite material, which comprises the steps of uniformly mixing graphene oxide powder and deionized water in proportion to obtain a suspension, mixing the suspension at the high temperature of 500-800 ℃ in an ammonia gas atmosphere, dissolving ammonia gas into deionized water to be alkaline, decomposing ammonia gas into nitrogen gas and hydrogen gas at the high temperature, using the nitrogen gas as a protective gas and the hydrogen gas as a reducing atmosphere, accelerating the reduction of the graphene oxide in the alkaline and high-temperature environment, enabling the reduced graphene to be more uniformly distributed in an AlSi10Mg matrix in the high-temperature environment, synchronously realizing the reducing atmosphere and the protective atmosphere by utilizing the decomposition of the ammonia gas in the high-temperature environment, ensuring the uniform proportion, completely reducing the prepared graphene-reinforced AlSi10Mg nano composite material graphene oxide, more uniformly distributing the graphene, and avoiding the agglomeration of the graphene by utilizing the deionized water to firstly mix, the interface bonding degree and wettability of the reinforcing phase and the matrix are higher, and the powder flowability is better.
A composite material printing and forming method is characterized in that the composite material is formed through a selective laser melting or electron beam melting technology, graphene in the composite material can play a role of a heterogeneous nucleating agent, and the nucleation rate in the solidification and crystallization process is improved. And the graphene can play a pinning role in a matrix, and the mechanical properties of the material are improved by means of the combined action of mechanisms such as dislocation density strengthening, Orowan strengthening, cleaning strengthening and the like by means of the lattice distortion, stacking faults, grain refinement, load transfer and the like at the interface joint. Therefore, when the composite powder is applied to metal additive manufacturing technologies such as Selective Laser Melting (SLM) and Electron Beam Melting (EBM), parts with more excellent performance can be prepared.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of graphene-enhanced AlSi10Mg nanocomposite powder according to an embodiment of the present invention.
Fig. 2 is an SEM image of graphene oxide powder in an embodiment of the present invention.
FIG. 3 is a TEM image of graphene oxide powder according to an embodiment of the present invention.
FIG. 4 is a graph comparing the flowability of composite powders prepared in examples 1-3 with the flowability of composite powders prepared by ball milling.
FIG. 5 is a graph comparing the tensile strength of the samples of examples 1-3 with the tensile strength of ball-milled powder-printed samples.
FIG. 6 is a graph comparing the yield strength of samples of examples 1-3 to the yield strength of ball-milled powder-printed samples.
FIG. 7 is a graph comparing the elongation of samples of examples 1-3 with the elongation of ball milled powder printed samples.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
it should be understood that the preferred embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the invention.
A preparation method of a graphene reinforced AlSi10Mg nanocomposite comprises the following steps:
s1, preparing a graphene oxide-deionized water suspension:
uniformly mixing graphene oxide powder and deionized water to obtain a turbid liquid A;
specifically, uniformly mixing graphene oxide powder and deionized water by adopting an ultrasonic oscillation method to obtain a graphene oxide-deionized water turbid liquid;
wherein the number of the thin film layers of the graphene oxide powder is 1-2, the particle size is 0.2-5nm, and the purity is 99.9%, as shown in fig. 2 and 3; the volume ratio of the mass of the graphene oxide powder to the deionized water is (1-20 mg): 1ml, and the time of ultrasonic oscillation is not less than 2 h.
S2, uniformly mixing the suspension A and the AlSi10Mg powder in an ammonia atmosphere at the mixing temperature of 500-800 ℃, and drying in a vacuum environment to obtain the graphene reinforced AlSi10Mg nanocomposite.
The grain diameter of the AlSi10Mg powder is micron-sized or nano-sized; the mass of the graphene oxide in the suspension A is 0.3-0.9% of that of the AlSi10Mg powder.
Specifically, firstly, a predetermined amount of graphene oxide-deionized water suspension and AlSi10Mg powder are loaded into a homogenizer, then ammonia gas is introduced, the flow rate of the ammonia gas is kept at 100-200ml/min, the revolution speed of the homogenizer is 10-30r/min, the self-transmission speed is 500-1500r/min, the temperature in the homogenizer is 500-800 ℃, and mixing is carried out for 5-15min, so that all reduced graphene of graphene oxide is ensured, and the graphene oxide is uniformly distributed in AlSi10Mg powder.
The temperature of vacuum drying is 110 ℃, and the time is not less than 12 h.
According to the invention, firstly, deionized water is used for mixing graphene oxide into a turbid liquid, then, the turbid liquid is mixed at the high temperature of 800 ℃ and in the atmosphere of ammonia gas, ammonia gas is dissolved into deionized water to be alkaline, the ammonia gas can be decomposed into nitrogen gas and hydrogen gas at the high temperature, the nitrogen gas is used as a protective gas, the hydrogen gas is used as a reducing atmosphere, the reduction of the graphene oxide can be accelerated in the alkaline and high-temperature environments, the reduced graphene can be more uniformly distributed in an AlSi10Mg matrix in the high-temperature environment, the reducing atmosphere and the protective atmosphere can be synchronously realized by the decomposition of the ammonia gas in the high-temperature environment, the proportion is uniform, the prepared graphene reinforced AlSi10Mg nano composite material graphene oxide is completely reduced, the graphene is more uniformly distributed, the interface bonding degree and the wettability of the reinforced phase and the matrix are higher, and the powder flowability is better.
Rotation with a homogenizer results in a more uniform distribution of graphene in the AlSi10Mg matrix.
Example 1
(1) AlSi10Mg powder is used as matrix powder, and the particle size is 15-53 μm. Taking the volume ratio of the mass of the graphene oxide powder to the deionized water as 5 mg: 1ml, the mass of the graphene oxide in the graphene oxide-deionized water suspension is 0.3% of the mass of the AlSi10Mg powder. 3g of graphene oxide was weighed and 600ml of deionized water was measured. Mixing for 2h by ultrasonic oscillation.
(2) 997g of AlSi10Mg powder was weighed and added to the homogenizer together with the graphene oxide-deionized water suspension. Setting the revolution speed of the homogenizer at 20r/min, the rotation speed of the homogenizer at 1000r/min, the flow of ammonia gas at 100ml/min and the temperature at 500 ℃. Mixing and reacting for 5min to obtain a mixture A.
(3) And (3) drying the mixture A in vacuum for 12h, setting the drying temperature to be 110 ℃, and drying to obtain the graphene reinforced AlSi10Mg nanocomposite.
(4) The powder was used to print samples using a selective laser melting technique and mechanical testing was performed.
The fluidity comparison graph of the graphene-reinforced AlSi10Mg composite material and the graphene-reinforced AlSi10Mg composite material prepared by ball milling is obtained, and the fluidity of the powder prepared by the method is obviously superior to that of the powder prepared by ball milling. The materials are used for selective laser melting, printing and forming, and a sample piece is tested to find that the tensile strength of the material reaches 492MPa, the yield strength reaches 322MPa, and the elongation reaches 9.5%.
Example 2
(1) AlSi10Mg powder is used as matrix powder, and the particle size is 15-53 μm. Taking the volume ratio of the mass of the graphene oxide powder to the deionized water as 10 mg: 1ml, the mass of the graphene oxide in the graphene oxide-deionized water suspension is 0.6% of the mass of the AlSi10Mg powder. 6g of graphene oxide was weighed and 600ml of deionized water was measured. Mixing for 2h by ultrasonic oscillation.
(2) 994g of alsi10Mg powder was weighed and added to the homogenizer together with the graphene oxide-deionized water suspension. Setting the revolution speed of the homogenizer at 20r/min, the rotation speed of the homogenizer at 1000r/min, the flow of ammonia gas at 100ml/min and the temperature at 500 ℃. Mixing and reacting for 5min to obtain a mixture A.
(3) And (3) drying the mixture A in vacuum for 12h, setting the drying temperature to be 110 ℃, and drying to obtain the graphene reinforced AlSi10Mg nanocomposite.
(4) The powder was used to print samples using a selective laser melting technique and mechanical testing was performed.
Example 3
(1) AlSi10Mg powder is used as matrix powder, and the particle size is 15-53 μm. Taking the volume ratio of the mass of the graphene oxide powder to the deionized water as 15 mg: 1ml, the mass of the graphene oxide in the graphene oxide-deionized water suspension is 0.9% of the mass of the AlSi10Mg powder. 9g of graphene oxide was weighed and 600ml of deionized water was measured. Mixing for 2h by ultrasonic oscillation.
(2) 991g of alsi10Mg powder was weighed and added to the homogenizer together with the graphene oxide-deionized water suspension. Setting the revolution speed of the homogenizer at 20r/min, the rotation speed of the homogenizer at 1000r/min, the flow of ammonia gas at 100ml/min and the temperature at 500 ℃. Mixing and reacting for 5min to obtain a mixture A.
(3) And (3) drying the mixture A in vacuum for 12h, setting the drying temperature to be 110 ℃, and drying to obtain the graphene reinforced AlSi10Mg nanocomposite.
(4) The powder was used to print samples using a selective laser melting technique and mechanical testing was performed.
In examples 1 to 3, AlSi10Mg powder was used as experimental powder, graphene reinforced composite powder was prepared by the method of the present invention, and the flowability of the powder prepared by ball milling and the powder prepared by in-situ generation according to the present invention and the mechanical properties of the samples printed with the two powders were compared, as shown in fig. 4 to 7, which are comparative graphs. It can be concluded that the fluidity of the composite metal powder prepared by the method (in-situ generation) is obviously superior to that of the composite metal powder prepared by the ball milling method, and the mechanical property of a sample prepared by the powder is also superior to that of a sample printed by the powder prepared by the ball milling.
Example 4
(1) AlSi10Mg powder is used as matrix powder, and the particle size is 15-53 μm. Taking the volume ratio of the mass of the graphene oxide powder to the deionized water as 5 mg: 1ml, the mass of the graphene oxide in the graphene oxide-deionized water suspension is 0.3% of the mass of the AlSi10Mg powder. 3g of graphene oxide was weighed and 600ml of deionized water was measured. Mixing for 2h by ultrasonic oscillation.
(2) 997g of AlSi10Mg powder was weighed and added to the homogenizer together with the graphene oxide-deionized water suspension. Setting the revolution speed of the homogenizer at 20r/min, the rotation speed of the homogenizer at 1000r/min, the flow of ammonia gas at 150ml/min and the temperature at 500 ℃. Mixing and reacting for 5min to obtain a mixture A.
(3) And (3) drying the mixture A in vacuum for 12h, setting the drying temperature to be 110 ℃, and drying to obtain the graphene reinforced AlSi10Mg nanocomposite.
Example 5
(1) AlSi10Mg powder is used as matrix powder, and the particle size is 15-53 μm. Taking the volume ratio of the mass of the graphene oxide powder to the deionized water as 10 mg: 1ml, the mass of the graphene oxide in the graphene oxide-deionized water suspension is 0.6% of the mass of the AlSi10Mg powder. 6g of graphene oxide was weighed and 600ml of deionized water was measured. Mixing for 2h by ultrasonic oscillation.
(2) 994g of alsi10Mg powder was weighed and added to the homogenizer together with the graphene oxide-deionized water suspension. Setting the revolution speed of the homogenizer at 20r/min, the rotation speed of the homogenizer at 1000r/min, the flow of ammonia gas at 150ml/min and the temperature at 500 ℃. Mixing and reacting for 5min to obtain a mixture A.
(3) And (3) drying the mixture A in vacuum for 12h, setting the drying temperature to be 110 ℃, and drying to obtain the graphene reinforced AlSi10Mg nanocomposite.
Example 6
(1) AlSi10Mg powder is used as matrix powder, and the particle size is 15-53 μm. Taking the volume ratio of the mass of the graphene oxide powder to the deionized water as 15 mg: 1ml, the mass of the graphene oxide in the graphene oxide-deionized water suspension is 0.9% of the mass of the AlSi10Mg powder. 9g of graphene oxide was weighed and 600ml of deionized water was measured. Mixing for 2h by ultrasonic oscillation.
(2) 991g of alsi10Mg powder was weighed and added to the homogenizer together with the graphene oxide-deionized water suspension. Setting the revolution speed of the homogenizer at 20r/min, the rotation speed of the homogenizer at 1000r/min, the flow of ammonia gas at 150ml/min and the temperature at 500 ℃. Mixing and reacting for 5min to obtain a mixture A.
(3) And (3) drying the mixture A in vacuum for 12h, setting the drying temperature to be 110 ℃, and drying to obtain the graphene reinforced AlSi10Mg nanocomposite.
Examples 4 to 6 the flow rate of ammonia gas was changed from 100ml/min to 150ml/min as compared with 1 to 3, in order to investigate the influence of the flow rate of ammonia gas on the original production reaction. The specific data and the corresponding estimated values of the mechanical properties of the printed samples are shown in the following table.
Graphene in the graphene-reinforced AlSi10Mg nano composite material can play a role of a heterogeneous nucleating agent, and the nucleation rate in the solidification and crystallization process is improved. And the graphene can play a pinning role in a matrix, and the mechanical properties of the material are improved by means of the combined action of in-situ dislocation density strengthening, Orowan strengthening and cleaning strengthening mechanisms by means of lattice distortion, stacking faults, grain refinement, load transfer and the like at interface joints. Therefore, when the composite powder is applied to metal additive manufacturing technologies such as Selective Laser Melting (SLM) and Electron Beam Melting (EBM), parts with more excellent performance can be prepared.
Claims (10)
1. A preparation method of a graphene reinforced AlSi10Mg nanocomposite is characterized by comprising the following steps:
s1, uniformly mixing graphene oxide powder and deionized water to obtain a suspension A, wherein the mass ratio of the graphene oxide powder to the volume ratio of the deionized water is (1-20 mg): 1 ml;
s2, uniformly mixing the suspension A and the AlSi10Mg powder in an ammonia atmosphere at the mixing temperature of 500-800 ℃, and drying in a vacuum environment to obtain the graphene reinforced AlSi10Mg nanocomposite.
2. The method for preparing the graphene-reinforced AlSi10Mg nanocomposite material according to claim 1, wherein the number of graphene oxide powder film layers is 1-2.
3. The preparation method of the graphene-reinforced AlSi10Mg nanocomposite material according to claim 1, wherein the graphene oxide powder has a particle size of 0.2-5nm and a purity of 99.9%.
4. The preparation method of the graphene-reinforced AlSi10Mg nanocomposite material according to claim 1, wherein the graphene oxide powder and deionized water are uniformly mixed by an ultrasonic oscillation method to obtain a graphene oxide-deionized water suspension.
5. The preparation method of the graphene-reinforced AlSi10Mg nanocomposite material according to claim 4, wherein the time of ultrasonic oscillation is not less than 2 h.
6. The method for preparing the graphene-reinforced AlSi10Mg nanocomposite as claimed in claim 1, wherein the AlSi10Mg powder has a particle size of micron or nanometer.
7. The method for preparing the graphene-reinforced AlSi10Mg nanocomposite material according to claim 1, wherein the mass of the graphene oxide in the suspension A is 0.3-0.9% of the mass of the AlSi10Mg powder.
8. The method as claimed in claim 1, wherein in step S2, the graphene-reinforced AlSi10Mg nanocomposite is prepared by firstly loading a predetermined amount of the graphene oxide-deionized water suspension and AlSi10Mg powder into a homogenizer, then introducing ammonia gas, and mixing for 5-15min while maintaining the flow rate of the ammonia gas at 200ml/min, the revolution speed of the homogenizer at 10-30r/min, the self-transmission speed at 1500r/min, and the temperature in the homogenizer at 500-800 ℃.
9. The preparation method of the graphene-reinforced AlSi10Mg nanocomposite material according to claim 1, wherein the temperature of vacuum drying is 110 ℃ and the time is not less than 12 h.
10. A method for printing and forming a composite material, characterized in that the composite material obtained in claim 1 is printed and formed by a selective laser melting technique or an electron beam melting technique.
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