阅读说明：本技术 一种铝基合金粉末及其制备方法、用途 (Aluminum-based alloy powder and preparation method and application thereof ) 是由 龚辉 沈益文 蔡亦恺 刘雨虹 于 2020-12-29 设计创作，主要内容包括：本发明涉及一种铝基合金粉末及其制备方法、用途。本发明的铝基合金粉末,含有铝基粉末、多层石墨烯以及多层石墨烯与铝基粉末进行合金化形成的组织；其中,所述铝基合金粉末的表面至少部分被多层石墨烯包覆。本发明中,用低成本的石墨代替了高成本的石墨烯为原料,利用球磨的均匀化作用和机械剥离作用,在分散剂的帮助下,利用真空环境干燥、并实现去除(或减少)铝基粉末中含氢、氧、氯化物等挥发性有害物质,实现高质量的石墨烯与铝基粉末的包覆与合金化。由于在制备过程中隔绝了空气,得到的成品减少了氧化物杂质污染,相对的品质更纯、润湿性更好,成本也相对较低。(The invention relates to aluminum-based alloy powder and a preparation method and application thereof. The aluminum-based alloy powder contains aluminum-based powder, multilayer graphene and a tissue formed by alloying the multilayer graphene and the aluminum-based powder; wherein the surface of the aluminum-based alloy powder is at least partially coated with multiple layers of graphene. According to the invention, low-cost graphite is used as a raw material instead of high-cost graphene, and the high-cost graphene is dried in a vacuum environment under the help of a dispersing agent by utilizing the homogenization effect and the mechanical stripping effect of ball milling, so that volatile harmful substances such as hydrogen, oxygen, chloride and the like in the aluminum-based powder are removed (or reduced), and the high-quality coating and alloying of the graphene and the aluminum-based powder are realized. Because air is isolated in the preparation process, the obtained finished product reduces the oxide impurity pollution, and has purer relative quality, better wettability and lower cost.)

1. The aluminum-based alloy powder is characterized by comprising aluminum-based powder, multilayer graphene and a tissue formed by alloying the multilayer graphene and the aluminum-based powder;

wherein the surface of the aluminum-based alloy powder is at least partially coated with multiple layers of graphene.

2. The aluminum-based alloy powder according to claim 1, wherein the average particle diameter of the aluminum-based alloy powder is 200 to 2000 mesh.

3. The aluminum-based alloy powder according to claim 1 or 2, wherein the mass ratio of the multilayer graphene to the aluminum-based powder in the aluminum-based alloy powder raw material is 1:20 to 1: 500.

4. The aluminum-based alloy powder according to claim 1 or 2, wherein the aluminum-based powder is an aluminum metal powder or an aluminum alloy powder.

5. A method for preparing an aluminium based alloy powder according to any of claims 1 to 4, comprising the steps of:

adding a solvent into graphite powder and aluminum-based powder to prepare a pasty liquid;

and (4) putting the pasty liquid into a ball mill, closing the container, and carrying out continuous treatment to obtain the aluminum-based alloy powder.

6. The method of claim 5, wherein the graphite powder is >99.9 wt% pure and flaky.

7. The production method according to claim 5 or 6, wherein the graphite powder is 3000 to 50000 mesh graphite powder, and the aluminum-based powder is 150 to 1500 mesh aluminum-based powder.

8. The method for the preparation according to claim 5 or 6, characterized in that said continuous treatment comprises the steps of:

step A), ball milling for 12-48 hours at normal temperature and normal pressure;

step B), vacuumizing and ball-milling for 2-10 hours at normal temperature;

step C), heating to 180-540 ℃ under vacuum, and simultaneously carrying out ball milling;

step D), preserving heat and performing ball milling for 2-12 hours in vacuum, wherein the pressure of the vacuum is less than 1 Pa;

and E), cooling, transferring to a vacuum tank for storage or directly using or filling protective gas for storage.

9. Use of the aluminium based alloy powder according to any one of claims 1 to 4 for 3D printing.

Technical Field

The invention relates to aluminum-based alloy powder and a preparation method thereof, belonging to the field of alloy materials.

Background

The aluminum matrix composite has excellent strength and rigidity, high temperature resistance and wear resistance, and low thermal expansion coefficient. At present, the reinforcing means of the aluminum matrix composite material adopts a fiber reinforcement body, which not only can improve the strength of the aluminum matrix composite material, but also can improve the plasticity of the aluminum matrix composite material.

Graphene is a novel two-dimensional material with the thickness of a monoatomic layer, is known to be the thinnest and the hardest nanometer material in the world, and therefore can be used as a filling material for modifying other materials. Due to the toughness, strength and surface activity of graphene, when used as a filler material, a chain bridge effect can be formed at a grain interface. The crystal grain interface of the base material is in a seamless connection form through the surface activity of the graphene. After the seamless connection is formed on the grain boundary in the base material, the grain boundary sliding phenomenon is reduced and the anti-stress capability is increased under the action of external force, so that the strength of the filled base material is enhanced along with the improvement of the anti-stress capability.

In the prior art, various forms of mixing processes are performed on finished graphene and aluminum particles. However, graphene has the problems of small size, large specific surface area, difficult dispersion and easy agglomeration, so that the existing graphene reinforced metal matrix composite material process has the problem of low yield and is difficult to realize large-scale production. Meanwhile, the production process of graphene is a complex, long-period and high-pollution process, and the conventional graphene is mainly produced in three ways: 1) mechanically stripping graphene; 2) carrying out chemical deposition on natural gas/methane gas and the like; 3) and reducing the graphite oxide. However, the existing graphene production processes have the following defects: the production process is long, the energy consumption is large, the environment is polluted, the cost is high, and the application of the composite material in enhancing other materials is limited.

Disclosure of Invention

Problems to be solved by the invention

In order to solve the above problems, the present invention provides an aluminum-based alloy powder and a method for preparing the same. According to the preparation method disclosed by the invention, the multilayer graphene can be fully dispersed in the aluminum-based alloy powder, meanwhile, the oxidation defect of the alloy can be prevented, and the high-quality and high-performance aluminum-based alloy powder can be obtained. The molded body obtained by using the aluminum-based alloy powder of the present invention has high tensile strength and high hardness.

Means for solving the problems

The invention provides an aluminum-based alloy powder, which contains aluminum-based powder, multilayer graphene and a tissue formed by alloying the multilayer graphene and the aluminum-based powder;

wherein the surface of the aluminum-based alloy powder is at least partially coated with multiple layers of graphene.

According to the aluminum-based alloy powder, the average particle size of the aluminum-based alloy powder is 200-2000 meshes.

According to the aluminum-based alloy powder, the mass ratio of the multi-layer graphene to the aluminum-based powder in the aluminum-based alloy powder raw material is 1: 20-1: 500.

According to the aluminum-based alloy powder of the present invention, the aluminum-based powder is aluminum metal powder or aluminum alloy powder.

The preparation method of the aluminum-based alloy powder comprises the following steps:

adding a solvent into graphite powder and aluminum-based powder to prepare a pasty liquid;

and (4) putting the pasty liquid into a ball mill, closing the container, and carrying out continuous treatment to obtain the aluminum-based alloy powder.

According to the aluminum-based alloy powder, the purity of the graphite powder is more than 99.9 wt%, and the graphite powder is flaky.

According to the aluminum-based alloy powder, the graphite powder is 3000-50000 meshes of graphite powder, and the aluminum-based powder is 150-1500 meshes of aluminum-based powder.

According to the aluminium-based alloy powder according to the invention, the continuous treatment comprises the following steps:

step A), ball milling for 12-48 hours at normal temperature and normal pressure;

step B), vacuumizing and ball-milling for 2-10 hours at normal temperature;

step C), heating to 180-540 ℃ under vacuum, and simultaneously carrying out ball milling;

step D), preserving heat and performing ball milling for 2-12 hours in vacuum, wherein the pressure of the vacuum is less than 1 Pa;

and E), cooling, transferring to a vacuum tank for storage or directly using or filling protective gas for storage.

The invention also provides the application of the aluminum-based alloy powder in 3D printing.

ADVANTAGEOUS EFFECTS OF INVENTION

According to the invention, low-cost graphite is used as a raw material instead of high-cost graphene, and the high-cost graphene is dried in a vacuum environment under the help of a dispersing agent by utilizing the homogenization effect and the mechanical stripping effect of ball milling, so that volatile harmful substances such as hydrogen, oxygen, chloride and the like in the aluminum-based powder are removed (or reduced), and the high-quality coating and alloying of the graphene and the aluminum-based powder are realized. Because air is isolated in the preparation process, the obtained finished product reduces the oxide impurity pollution, and has purer relative quality, better wettability and lower cost.

Drawings

FIG. 1: scanning electron microscope picture of the aluminum-based alloy powder-I obtained in example 1.

FIG. 2: scanning electron microscope picture of the aluminum-based alloy powder-II obtained in example 2.

FIG. 3: scanning electron microscope pictures of aluminum powder without graphite addition.

Detailed Description

The present invention will be described in detail below. The technical features described below are explained based on typical embodiments and specific examples of the present invention, but the present invention is not limited to these embodiments and specific examples. It should be noted that:

in the present specification, the numerical range represented by "numerical value a to numerical value B" means a range including the end point numerical value A, B.

In the present specification, "plural" in "plural", and the like means a numerical value of 2 or more unless otherwise specified.

In this specification, the terms "substantially", "substantially" or "substantially" mean an error of less than 5%, or less than 3% or less than 1% as compared to the relevant perfect or theoretical standard.

In the present specification, "%" denotes mass% unless otherwise specified.

In the present specification, the meaning of "may" includes both the meaning of performing a certain process and the meaning of not performing a certain process.

In this specification, "optional" or "optionally" means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where the event occurs and instances where it does not.

In the present specification, reference to "some particular/preferred embodiments," "other particular/preferred embodiments," "embodiments," and the like, means that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described elements may be combined in any suitable manner in the various embodiments.

The invention provides an aluminum-based alloy powder, which contains aluminum-based powder, multilayer graphene and a tissue formed by alloying the multilayer graphene and the aluminum-based powder;

wherein the surface of the aluminum-based alloy powder is at least partially coated with multiple layers of graphene.

According to the aluminum-based alloy powder, the average particle size of the aluminum-based alloy powder is 200-2000 meshes.

According to the aluminum-based alloy powder, the mass ratio of the multi-layer graphene to the aluminum-based powder in the aluminum-based alloy powder raw material is 1: 20-1: 500.

According to the aluminum-based alloy powder of the present invention, the aluminum-based powder is aluminum metal powder or aluminum alloy powder.

The invention also provides a preparation method of the aluminum-based alloy powder, which comprises the following steps:

adding a solvent into graphite powder and aluminum-based powder to prepare a pasty liquid;

and (4) putting the pasty liquid into a ball mill, closing the container, and carrying out continuous treatment to obtain the aluminum-based alloy powder.

According to the preparation method, the purity of the graphite powder is more than 99.9 wt%, and the graphite powder is flaky.

According to the preparation method, the graphite powder is 3000-50000 meshes of graphite powder, and the aluminum-based powder is 200-800 meshes of aluminum-based powder.

According to the preparation method of the invention, the continuous treatment comprises the following steps:

step A), ball milling for 12-48 hours at normal temperature and normal pressure;

step B), vacuumizing and ball-milling for 2-10 hours at normal temperature to remove the solvent;

step C), heating to 180-540 ℃ under vacuum, and simultaneously carrying out ball milling;

step D), preserving heat and carrying out ball milling for 2-12 hours in vacuum, wherein the pressure of the vacuum is less than 1 Pa;

and E), cooling, transferring to a vacuum tank for storage or directly using.

Examples

Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.

Example 1

3g of 800-mesh graphite powder with the purity of 99.9 wt% and 600g of 500-mesh 1060-mesh aluminum powder are used as raw materials to be mixed, and then a proper amount of 99% absolute ethyl alcohol is added to prepare a pasty solution, wherein the mass ratio of the material liquid is about 1: 10.

Putting the solution into an all-in-one machine for ball milling, vacuum drying and heat treatment, adding stainless steel balls (ball material mass ratio is 12:1), closing a container, and carrying out continuous treatment.

The continuous treatment process comprises the following steps:

A) ball milling is carried out for 12 hours at normal temperature and normal pressure;

B) gradually pumping to vacuum at normal temperature and ball-milling for 2 hours;

C) heating at 1 degree/min and gradually vacuumizing and ball-milling to 460 ℃;

D) ball milling at 460 ℃ under vacuum (<1Pa) for 2 hours;

E) cooling and transferring to a vacuum tank for storage to obtain the aluminum-based alloy powder-I.

Example 2

30g of graphite powder with the purity of 99.9 wt% of 300 meshes and 600g of 1060 aluminum powder with the purity of 500 meshes are used as raw materials to be mixed, and then a proper amount of 99% absolute ethyl alcohol is added to prepare a pasty solution, wherein the mass ratio of the material liquid is about 1: 10.

Putting the solution into an all-in-one machine for ball milling, vacuum drying and heat treatment, adding stainless steel balls (ball material mass ratio is 12:1), closing a container, and carrying out continuous treatment.

The continuous treatment process comprises the following steps:

A) ball milling is carried out for 16 hours at normal temperature and normal pressure;

B) gradually pumping to vacuum at normal temperature and ball-milling for 2 hours;

C) heating at 0.5 deg.c/min while vacuum ball milling to 400 deg.c;

D) ball milling at 400 ℃ under vacuum (<1Pa) for 2 hours;

E) cooling and transferring to a vacuum tank for storage to obtain aluminum-based alloy powder-II.

Application example 1

And (3) continuously carrying out hot isostatic pressing on the aluminum-based alloy powder-I obtained in the example 1 to obtain an aluminum-olefin alloy-I, and carrying out a performance test on the aluminum-olefin alloy-I.

Comparative application example 1

The aluminum powder with the same composition and without graphite addition as that used in example 1 was subjected to hot isostatic pressing to obtain aluminum alloy-I, and the aluminum-olefin alloy-I obtained in application example 1 had a tensile strength of 342/221MPa, which was increased by 55% as compared with aluminum alloy-I.

Application example 2

The aluminum-based alloy powder-II obtained in example 2 is hot extruded into an aluminum-olefin alloy wire, and the aluminum-olefin alloy-II can be obtained by normal state storage after continuous extrusion into a wire without cooling.

Comparative application example 2

The aluminum powder with the same composition as that used in example 2 and without graphite addition was hot extruded into aluminum wire, and was continuously extruded into wire without cooling to obtain aluminum alloy-II.

The aluminum alloy is cast by adopting the alloy composition with the same components, the aluminum alkene alloy-II and the aluminum alloy-II are respectively used as intermediate alloys, the addition amount of 0.5 wt% of the intermediate alloys is added into the aluminum molten liquid to produce the aluminum alloy, and the tensile strength of the aluminum alloy after the aluminum alkene alloy-II is added is improved by 27% compared with that of the aluminum alloy-2.

Application example 3

The aluminum-based alloy powder-I obtained in example 1 is used as a 3D printing material, and a 3D printer is used for printing a test piece which is marked as an aluminum-olefin alloy 3D-I.

Comparative application example 3

The same aluminum powder as that used in example 1, which was not added with graphite, was used as a 3D printing material, and a test piece was printed out with a 3D printer and recorded as aluminum alloy 3D-I.

Compared with the aluminum alloy 3D-I, the tensile strength of the aluminum-olefin alloy 3D-I obtained in the application example 3 is 374/231MPa, which is improved by 62%.

Application example 4

The aluminum-based alloy powder-II obtained in the example 2 is used as a 3D printing material, and a test piece is printed by a 3D printer and is marked as an aluminum-olefin alloy 3D-II.

Comparative application example 4

The same aluminum powder as used in example 2 without graphite addition was used as a 3D printing material, and a test piece was printed out with a 3D printer and recorded as aluminum alloy 3D-II.

The aluminum alloy 3D-II obtained in application example 4 had hardness increased from HB90 to HB147, compared with the aluminum alloy 3D-II.

It should be noted that, although the technical solutions of the present invention are described in specific embodiments, those skilled in the art can understand that the present invention should not be limited thereto.

Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.