CN112916142B - Planetary ball milling-based liquid metal material mixing process - Google Patents
Planetary ball milling-based liquid metal material mixing process Download PDFInfo
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- CN112916142B CN112916142B CN202110127811.8A CN202110127811A CN112916142B CN 112916142 B CN112916142 B CN 112916142B CN 202110127811 A CN202110127811 A CN 202110127811A CN 112916142 B CN112916142 B CN 112916142B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
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Abstract
The invention relates to a mixing process of liquid metal materials based on planetary ball milling, which comprises the steps of placing liquid metal and solid materials into ball milling equipment, and carrying out ball milling treatment under the shearing action of a ball milling medium to finish uniform dispersion. Compared with the prior art, the invention realizes the uniform dispersion between the materials and the liquid metal by the liquid metal material mixing process based on planetary ball milling, realizes the preparation process of mixing the liquid metal and the materials to be mixed under the specified temperature, pressure and atmosphere environment, breaks through the application limit that common materials can not be wetted with the liquid metal, has wide application range, and can be used for various purposes such as metal coating, composite material preparation, structural design and the like.
Description
Technical Field
The invention belongs to the technical field of novel functional materials, and relates to a planetary ball milling-based liquid metal material mixing process.
Background
The liquid metal has a great prospect in the fields of wearable devices, microelectronics, biomedicine and the like, and has important significance in the preparation and structural design of composite materials of the liquid metal. At present, the mode of mixing liquid metal and materials is only limited to manual grinding and electric stirring, and the phenomenon of uneven dispersion exists. Meanwhile, due to the non-wetting phenomenon between most of the materials and the liquid metal, the mixing of the materials and the liquid metal has limitation, and research on the performance change caused by the mixing of the liquid metal and other materials is limited. Therefore, it is very important how to improve the wetting property of liquid metal and other materials.
Disclosure of Invention
The invention aims to provide a mixing process of liquid metal materials based on planetary ball milling.
The purpose of the invention can be realized by the following technical scheme:
a mixing process of liquid metal materials based on planetary ball milling is characterized in that liquid metal and solid materials are placed in ball milling equipment, and ball milling treatment is carried out under the shearing action of a ball milling medium, so that uniform dispersion is completed.
Further, the liquid metal is metallic mercury, gallium-indium alloy, gallium-indium-tin alloy, metallic gallium or metallic rubidium.
Further, the solid material is graphite powder, copper particles, boron nitride, nickel powder, graphene or diamond particles.
Furthermore, the ball milling medium is ball milling beads, and the material of the ball milling beads is zirconia, alumina or silicon carbide.
Further, the particle size of the ball milling beads is not more than 10 mm, and the particle size of the solid material is in the order of micrometer to millimeter.
Further, gas which is partially reacted with the liquid metal or the solid material is introduced in the ball milling process so as to introduce the modified chemical functional groups at the edge of the liquid metal or the solid material. More preferably, the gas may be air, oxygen, chlorine, or the like.
Furthermore, in the ball milling treatment, the solid material can simultaneously introduce functional groups such as modified chemical functional groups of hydroxyl, carboxyl, aldehyde and the like under the mechanochemical shearing action of a ball milling medium.
Furthermore, the temperature of the ball milling treatment is below the boiling point temperature of the liquid metal and above the supercooling temperature.
Furthermore, a solvent is added in the ball milling treatment process.
Further, the solid material is in the form of powder, granule, tablet, block or microsphere.
The invention uses the mechanical shearing force of the ball milling media ball milling beads to impact the materials to be mixed with certain strength and has the function of dispersing the materials. In the ball-milling process, the ball-milling medium passes through mechanochemical's shearing action, on the one hand can do benefit to the granularity reduction of solid material and mix with liquid metal, on the other hand the shearing force of ball-milling medium can be extremely fast constantly on the surface of the liquid metal droplet of breaing up and produce the oxide layer, and the oxide layer is the prerequisite that solid filler sneaks into liquid metal, compare in conventional stirring mixed mode, the speed that this kind of method produced the oxide layer on liquid metal surface has far exceeded traditional mode, make solid filler can be more quick carry out abundant even mixture with liquid metal, the efficiency and the effect of mixing have all obtained great promotion.
Compared with the prior art, the invention has the following advantages:
(1) the invention realizes uniform dispersion between the liquid metal and the material by the planetary ball milling process of the liquid metal and the material, and has wide application range.
(2) The invention breaks through the application limit that common materials can not be mutually wetted with the liquid metal, realizes the preparation process of mixing the liquid metal and the material to be mixed under the specified temperature, pressure and atmosphere environment, and has wider research value and application prospect.
(3) The invention is not influenced by the shape, size, viscosity, surface tension and other properties of specific materials, and has wide application range.
(4) The preparation method is simple, has various adjustable modes and high repeatability, can be used for obtaining final products with different ideal effects, and is convenient for realizing large-scale production.
(5) The invention can realize surface chemical modification of materials while ball milling, and is used for multiple purposes such as metal coating, composite material preparation, structural design and the like, which cannot be achieved by the prior art.
Drawings
FIG. 1 is a schematic process diagram of a ball milling process of the present invention;
FIG. 2 is a scanning electron microscope photograph of the final product after ball milling of gallium and graphite;
FIG. 3 is a graph showing the variation of thermal and electrical properties after ball milling of gallium metal and graphite;
FIG. 4 is a diagram showing the mixing state of gallium metal and graphite obtained in example 1 and a conventional mixing process;
FIG. 5 is a graph of infrared data of a ball milled final product of example 1 with pure gallium metal and graphite;
FIG. 6 is a comparison of the mixing state of the ball-milled final product of example 1 and the product obtained under the same process conditions under vacuum conditions;
FIG. 7 is the thermal conductivity of the final product of the Ga-in alloy prepared in example 2 after ball milling of the copper ball particles with different volume fractions;
FIG. 8 shows the morphology of the ball-milled final product of example 2 and the mixing state of the gallium-indium alloy and the copper ball particles for the same specification parameters of the conventional mixing process;
FIG. 9 is the thermal conductivity of the gallium metal prepared in example 3 after ball milling of the boron nitride powder with different volume fractions;
fig. 10 shows the morphology of the ball milled end product of example 3 and the state of mixing of metallic gallium and boron nitride powders for the same specification parameters for the conventional mixing process.
The notation in the figure is:
1-ball milling tank, 2-ball milling medium, 3-solid material and 4-liquid metal.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The ball milling and mixing process of the present invention will be explained.
The invention provides a mixing process of liquid metal materials based on planetary ball milling, which comprises the steps of placing liquid metal and solid materials into ball milling equipment, and carrying out ball milling treatment under the shearing action of a ball milling medium to finish uniform dispersion.
In some embodiments, the liquid metal is metallic mercury, gallium indium alloy, gallium indium tin alloy, metallic gallium, or metallic rubidium.
In some embodiments, the solid material is graphite powder, copper particles, or diamond particles.
In some embodiments, the ball milling media are ball milling beads made of zirconia, alumina, or silicon carbide.
Further, the particle size of the ball milling beads is not more than 10 mm, and the particle size of the solid material is in the order of micrometer to millimeter.
In some embodiments, a gas is also introduced that partially reacts with the liquid metal or solid material to introduce modifying chemical functionality, such as air, oxygen, chlorine, etc., at the edges of the liquid metal or solid material.
Furthermore, in the ball milling treatment, the solid material can simultaneously introduce functional groups such as modified chemical functional groups of hydroxyl, carboxyl, aldehyde and the like under the mechanochemical shearing action of a ball milling medium.
In some embodiments, the temperature of the ball milling process is below the boiling temperature of the liquid metal and above the supercooling temperature.
In some embodiments, a solvent is also added during the ball milling process.
In some embodiments, the solid material is in the form of a powder, granules, flakes, chunks, or microspheres.
The above embodiments may be implemented individually, or in any combination of two or more.
The above embodiments will be described in more detail with reference to specific examples.
Example 1
The ball milling equipment of this embodiment is as shown in fig. 1, and mainly includes a ball milling tank and a ball milling medium 2 disposed in the ball milling tank 1, and during operation, solid material 3 and liquid metal 4 are added into the ball milling tank 1, and under the air condition, the operation parameters are adjusted to perform ball milling, that is, the uniform mixing of the two is realized. The specific process is as follows:
(1) adding 10g of liquid metal gallium into a ball milling tank, adding 0.2g of graphite powder with the sheet diameter of 3-6 mu m, adding 12g of zirconium dioxide ball milling beads with the diameter of 2mm serving as ball milling media, and placing the ball milling media in a planetary ball mill under the air condition for ball milling.
(2) Referring to fig. 1, the rotation speed of the ball mill is set to be 400rpm, the ball milling time is set to be 3h, and the operation mode is non-turnover operation. After ball milling, a vacuum drying process is adopted to remove dense cavities in the composite material in the ball milling process. Vacuum drying at 20 deg.c for 3 hr to obtain the final liquid metal composite material.
Fig. 2 shows a scanning electron microscope photograph of the final product after ball milling of metal gallium and graphite prepared as described above, and it can be seen that the dispersion between the metal gallium and graphite is uniform and stable by the above process.
Fig. 3 shows the graph of the thermal and electrical property changes of the metal gallium after ball milling the graphite powder with different quality by the same process, and it can be seen that the thermal conductivity of the final product of the metal gallium and the graphite after ball milling is improved, and the electrical conductivity of the product based on the liquid metal gallium is almost unchanged.
Fig. 4 shows the morphology of the final ball-milled product obtained by the process and the mixing state of the conventional mixing process for the gallium metal and the graphite with the same specification parameters, and it can be seen that the effect of ball-milling mixing is more uniform.
Fig. 5 shows an infrared data diagram of the final product of ball milling obtained by the process, pure gallium and graphite, and it can be seen that an infrared peak at 3319cm-1 shows that the graphite is subjected to chemical modification by edge milling, functional groups of carboxyl and hydroxyl are introduced to form hydrogen bonds with a liquid metal oxide layer, so that the interaction force with the liquid metal is enhanced, and the product is more stable.
Fig. 6 shows a comparison graph of a ball-milling final product obtained by the process and a product obtained under the vacuum condition under the same process conditions, and it can be seen that chemical functional groups such as hydrogen bonds are introduced into the edge of liquid metal gallium under the atmosphere conditions such as air and oxygen, so that better mixing and dispersion with graphite can be realized.
Example 2
By using the ball milling device as in example 1, in this example, 10g of liquid metal gallium indium alloy, 1g of copper ball particles, and 10g of zirconium dioxide ball milling beads with a diameter of 2-3mm were taken as the ball milling media and placed in a ball milling tank. And performing ball milling under the air condition, wherein the ball milling time is set to be 1 h. The rest is the same as in example 1.
Fig. 7 shows the data of the thermal conductivity of the final product after ball milling of the gallium-indium alloy on the copper ball particles with different volume fractions, and it can be seen that, through the above process, the thermal conductivity of the final product after ball milling of the gallium-indium alloy on the copper ball particles with different volume fractions is improved along with the addition of the copper particles.
Fig. 8 shows the morphology of the final ball-milled product obtained by the process and the mixing state of the gallium-indium alloy and the copper ball particles with the same specification parameters in the conventional mixing process, and it can be seen that the ball-milling mixing effect is more uniform.
Example 3
The liquid metal gallium and the solid material in the example 1 are replaced by boron nitride powder, and the liquid metal gallium and the solid material are ball-milled with 10g of zirconium dioxide ball-milling beads with the diameter of 2-3mm for 2 hours under the air condition, so that the uniformly dispersed mixed material of the liquid metal and the boron nitride is prepared.
Fig. 9 shows the data of the thermal conductivity of the final product of ball milling of the boron nitride powder with different volume fractions by the prepared metal gallium, and it can be seen that, by the above process, the overall thermal performance changes with the addition of the boron nitride powder.
Fig. 10 shows the morphology of the ball-milled final product obtained by the process and the mixing state of the metal gallium and boron nitride powder with the same specification parameters of the conventional mixing process, and it can be seen that the ball-milling mixing effect is more uniform.
Example 4
Using the ball milling apparatus as in example 1, 10g of liquid metal gallium indium alloy, 1g of diamond particles, and 10g of zirconium dioxide ball milling beads having a diameter of 2 to 3mm were placed in a ball milling jar as a ball milling medium. Under the air condition, the operation mode is set to be turnover operation. The rest is the same as in example 1.
In the above examples, the conventional mixing process is a conventional electric stirring process, and the rest of the raw materials or treatment techniques, which are not specifically described, are conventional commercially available raw materials or conventional treatment techniques in the art.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. A mixing process of liquid metal materials based on planetary ball milling is characterized in that the liquid metal and solid materials are placed in ball milling equipment and are subjected to ball milling treatment under the shearing action of a ball milling medium, and uniform dispersion is completed;
gas which partially reacts with the liquid metal or the solid material is also introduced in the ball milling process so as to introduce modification chemical functional groups at the edge of the liquid metal or the solid material;
the gas is air, oxygen or chlorine; the liquid metal is metallic mercury, gallium-indium alloy, gallium-indium-tin alloy, metallic gallium or metallic rubidium;
the solid material is graphite powder, copper particles, boron nitride, nickel powder, graphene or diamond particles;
the chemical functional group is hydroxyl, carboxyl or aldehyde group.
2. The mixing process of the liquid metal material based on the planetary ball milling as claimed in claim 1, wherein the ball milling media are ball milling beads made of zirconia, alumina or silicon carbide.
3. A process for mixing a liquid metal material based on planetary ball milling according to claim 2, characterized in that the particle size of said ball milling beads does not exceed 10 mm and the particle size of the solid material is in the order of micron to mm.
4. The mixing process of liquid metal materials based on planetary ball milling according to claim 1, characterized in that the temperature of ball milling process is below the boiling temperature of liquid metal and above the supercooling temperature.
5. The mixing process of a liquid metal material based on planetary ball milling according to claim 1, wherein a solvent is further added during the ball milling process.
6. The mixing process of a liquid metal material based on planetary ball milling according to claim 1, characterized in that the solid material is in the form of powder, granules, flakes, blocks or microspheres.
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