CN114632936A - Multistage gradient ball milling method prepared by compounding nano phase and metal powder - Google Patents
Multistage gradient ball milling method prepared by compounding nano phase and metal powder Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a multistage gradient ball milling method for composite preparation of a nano phase and metal powder. The ball milling method of the invention comprises the following steps: performing ball milling on the nano-phase powder and the metal powder at a multi-stage ball milling rotating speed which is gradually increased from low to high to prepare composite powder, and overcoming the processing hardening generated by the ball milling deformation of the metal powder through multi-stage gradient regulation of the ball milling rotating speed; on one hand, the metal powder is fully fragmented along with the ball milling process, the surface area of the metal powder is maximized, and the nano-phase is promoted to be uniformly dispersed on the surface of the fragmented metal powder, so that nano-phase/metal flaky composite powder is obtained; on the other hand, once the metal powder does not have plastic deformation capacity any more and sheet metal powder is crushed in the ball milling process, the high-speed ball milling at a continuously increased rotating speed slowly welds the nano-phase/metal sheet composite powder to obtain the nano-phase/metal particle composite powder. The ball milling method of the invention can solve the problems of uniform dispersion and interface combination of the nano phase in the metal powder.
Description
Technical Field
The invention relates to a multistage gradient ball milling method for preparing a nano phase and metal powder in a composite mode, and belongs to the technical field of preparation of metal-based composite materials.
Background
In recent years, nano-reinforcing technology has become one of the important methods for improving mechanical and functional properties of metal materials. The nanophase enhanced metal matrix composite material has widely attracted attention in the fields of electronics, automobiles, ships, metallurgy and aerospace due to superior mechanical, electrical, thermal, optical and magnetic properties. How to prepare the nano-phase reinforced metal matrix composite with better performance is an urgent requirement in the technical field of the preparation of the current metal matrix composite. An important factor influencing the performance of the nano-phase reinforced metal matrix composite is the distribution characteristics and structural characteristics of the nano-phase in the metal matrix.
Since the 70 s, mechanical ball milling of powder particles has become an important method for the industrial synthesis of new alloys and new materials for multiphase mixtures, also known as mechanical alloying. The powder metallurgy technology can be used for preparing alloy and composite materials which cannot be obtained by the conventional smelting and casting technology, is suitable for large-scale production, and is a material preparation method with low price, environmental friendliness, high efficiency and high controllability. However, in the nano-phase/metal composite material prepared by the conventional mechanical ball milling method, the dispersibility and structural integrity of the nano-phase are poor, the nano-phase is easy to agglomerate, and the structure of the nano-phase is damaged to a certain extent, so that the reinforcing effect of the nano-phase cannot be fully exerted, and the performance of the composite material is restricted.
At present, researchers mainly focus on the influence of single ball milling time, ball milling rotating speed or coupling factors of the ball milling time and the ball milling rotating speed on the mechanical ball milling process; but the overall effect is not good, the nano-phase is difficult to be firmly welded with the matrix while ensuring the uniform distribution and the complete structure of the nano-phase, and the defects are few. The nano-phase in the composite powder prepared by low-speed ball milling is dispersed on the surface of the powder, the combination is weaker, and the flake powder has small loose volume, poor deformation and difficult densification. The nano phase in the composite powder prepared by high-speed ball milling is not enough to be dispersed fully, and the metal powder is rapidly flaked and welded. The patent "powder metallurgy preparation method of nanophase/metal composite powder and block material thereof" (CN 106363185a) discloses a powder metallurgy preparation method of nanophase/metal composite powder and block material thereof, which comprises the steps of firstly carrying out long-time low-speed ball milling on nanophase powder and metal powder to flake the metal powder, and simultaneously uniformly dispersing nanophase on the surface or inside the flaky metal powder to obtain nanophase/metal flake composite powder; and then the nano-phase/metal flake composite powder is welded together by short-time high-speed ball milling to obtain the nano-phase/metal granular composite powder. However, such variable speed ball milling process parameters (such as rotation speed and time) are not easy to control, and the metal powder gradually undergoes work hardening during the ball milling process, and the plastic deformation capability of the metal powder is weakened until the metal powder is lost, so that the powder preparation effect is affected and the process is time-consuming.
Disclosure of Invention
The technical problem solved by the invention is as follows: when the nano-phase/metal composite material is prepared by the existing ball milling process, the nano-phase/metal composite material is difficult to be firmly welded with a matrix while ensuring the uniform distribution and the complete structure of the nano-phase, or the metal powder is gradually processed and hardened in the ball milling process, the plastic deformation capability of the metal powder is weakened until the metal powder is lost, so the powder preparation effect is influenced, the time consumption of the process is high, and the like.
In order to solve the technical problems, the invention provides a multistage gradient ball milling method for preparing a nano phase and metal powder in a composite way, which comprises the following steps: performing ball milling on the nano-phase powder and the metal powder at a multi-stage ball milling rotating speed which is gradually increased from low to high to prepare composite powder, and overcoming the processing hardening generated by the ball milling deformation of the metal powder through multi-stage gradient regulation of the ball milling rotating speed;
wherein the ball milling rotating speeds of the multiple stages are n stages, n is an integer larger than or equal to 2, and the ball milling rotating speeds of the first stage to the nth stage are sequentially set as r1～rnSetting the ball milling time corresponding to the ball milling rotation speed of each stage as t1～tn(ii) a The ball milling rotating speed needs to meet the following conditions: r is not more than 10rpm1～rnR is not less than 1000rpm and not less than 5rpmn-rn-1The speed is less than or equal to 100rpm, and the ball milling time needs to meet the conditions as follows: t is more than or equal to 0.5h1～tn≤5h。
Preferably, the nanophase comprises nano-carbon nanotubes, nano-carbon spheres, nano-carbon fibers, nano-carbon sheets, nano-carbon onions, graphene and graphene oxideRedox graphene, nanodiamond, nano SiC and nano B4C. Nano WC and nano Al2O3Nano ZnO and nano TiO2Nano SiO2Nano ZrO 22Nano AlN, nano TiN and nano TiB2At least one of (1).
Preferably, the metal powder includes at least one of Al, Cu, Mg, Ti, Fe, Ni, Zn, Zr, Cr, Co, and W or an alloy powder thereof.
Preferably, the mass fraction of the nano phase is 0.005-30% of the composite powder.
Preferably, the material-ball ratio in the ball milling process is 1: 2-100, and the diameter of the milling ball is 2-120 mm.
Preferably, the ball milling process requires the addition of process control agents; the process controller is at least one of methanol, ethanol, titanate, silicone oil, oleic acid, imidazoline, paraffin, cellulose and stearic acid
In the multistage gradient ball milling method, the ball milling rotating speed is designed to be gradually increased from low-speed ball milling to high-speed ball milling and is changed in multistage gradient rotating speed, the corresponding different ball milling rotating speeds can be continuously the same or different time, and the deformation hardening generated by the ball milling deformation of the metal powder is overcome through multistage gradient regulation and control of the rotating speed. On one hand, the metal powder is fully fragmented along with the ball milling process, the surface area of the metal powder is maximized, and the nano-phase is promoted to be uniformly dispersed on the surface of the fragmented metal powder, so that nano-phase/metal flaky composite powder is obtained; on the other hand, once the metal powder does not have plastic deformation capacity any more in the ball milling process, the flaky metal powder is crushed, and the high-speed ball milling at the rotating speed is continuously improved to slowly weld the nano-phase/metal flaky composite powder to obtain the nano-phase/metal particle composite powder.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the multistage gradient ball milling method for preparing the nano phase and the metal powder in a composite mode, the problems of uniform dispersion and interface combination of the nano phase in the metal powder can be solved by adjusting the ball milling speed in a multistage gradient mode, and compared with the traditional uniform-speed ball milling, the nano phase is more uniform in dispersion and higher in interface combination strength; the sampling observation of the quality of the composite powder under different ball milling rotating speeds is facilitated, and the optimization and upgrading of the process are facilitated;
2. compared with the existing variable speed ball milling method, the invention can obviously improve the ball milling efficiency through the multi-level gradient regulation and control of the rotating speed, saves energy and time, simultaneously has slow powder welding, generates small processing strain gradient, is not easy to crush the sheet-shaped powder, and improves the quality of the composite powder;
3. the multistage gradient ball milling method for preparing the nano phase and the metal powder in a compounding way adopts diversified and extensive regulation and control of parameters such as rotating speed, time and the like in the ball milling process at each stage, widens the applicability of raw materials, and can be used for compounding various metal powder, alloy powder and nano phase materials.
Drawings
FIG. 1 is a scanning electron microscope image of the carbon nanotube/aluminum composite powder prepared in example 1 at scales of 200 μm (a), 50 μm (b), and 40 μm (c), respectively;
FIG. 2 is a scanning electron microscope image of the carbon nanotube/aluminum composite powder prepared in comparative example 1 at scales of 100 μm (a) and 500nm (b), respectively;
FIG. 3 is a scanning electron microscope image of the carbon nanotube/aluminum composite powder prepared in comparative example 2 at scales of 100 μm (a) and 2 μm (b), respectively;
FIG. 4 is a scanning electron microscope image of the carbon nanotube/aluminum composite powder prepared in comparative example 3 at scales of 200 μm (a), 50 μm (b), and 10 μm (c), respectively;
FIG. 5 is a scanning electron microscope image of the nano-SiC/Al composite powder prepared in example 2 at scales of 100 μm (a) and 10 μm (b), respectively;
FIG. 6 is a scanning electron micrograph of the graphene/copper composite powder prepared in example 3 at scales of 200 μm (a), 100 μm (b), and 30 μm (c), respectively.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Example 1
Carbon nanotube/aluminum composite powder
Spherical aluminum powder with the purity of more than 99.5 percent and the average particle size of 10 microns is used as metal matrix powder, multi-walled carbon nanotubes with the outer diameter of 20-40 nanometers and the length of 2-5 microns are used as nano-phase powder, and the mass fraction of the carbon nanotubes is 2 percent.
Placing the carbon nano tube/aluminum mixed powder into a planetary ball mill, wherein the ball-material ratio is 20:1, adding stearic acid with the mass fraction of 1%, wherein the multistage gradient ball milling process parameters are as follows: r is1＝135rpm，r2＝160rpm，r3＝185rpm，r4＝210rpm，r5＝230rpm，r6＝250rpm，r7＝270rpm；t1＝1h，t2＝1h，t3＝1h，t4＝1h，t5＝1h，t6＝1h，t7The scanning electron microscope results of the carbon nanotube/aluminum granular composite powder obtained after 1h are shown in fig. 1.
Comparative example 1
Carbon nanotube/aluminum composite powder
The same spherical aluminum powder with the purity of more than 99.5 percent and the average particle size of 10 microns as that in example 1 is used as metal matrix powder, multi-walled carbon nanotubes with the outer diameter of 20-40 nanometers and the length of 2-5 microns are used as nano-phase powder, and the mass fraction of the carbon nanotubes is 2 percent.
Placing the carbon nano tube/aluminum mixed powder in a planetary ball mill with a ball-material ratio of 20:1, adding stearic acid with the mass fraction of 1%, and ball-milling at the rotating speed of 135rpm for 9 hours to prepare the carbon nano tube/aluminum granular composite powder, wherein the scanning electron microscope result is shown in figure 2.
Comparative example 2
Carbon nanotube/aluminum composite powder
The same spherical aluminum powder with the purity of more than 99.5 percent and the average particle size of 10 microns as that in example 1 is used as metal matrix powder, multi-walled carbon nanotubes with the outer diameter of 20-40 nanometers and the length of 2-5 microns are used as nano-phase powder, and the mass fraction of the carbon nanotubes is 2 percent.
Placing the carbon nanotube/aluminum mixed powder in a planetary ball mill with a ball-to-material ratio of 20:1, adding stearic acid with a mass fraction of 1%, and ball-milling at 270rpm for 9h to prepare carbon nanotube/aluminum granular composite powder, wherein the scanning electron microscope result is shown in fig. 3.
Comparative example 3
Carbon nanotube/aluminum composite powder
The same spherical aluminum powder with the purity of more than 99.5 percent and the average particle size of 10 microns as that in example 1 is used as metal matrix powder, multi-walled carbon nanotubes with the outer diameter of 20-40 nanometers and the length of 2-5 microns are used as nano-phase powder, and the mass fraction of the carbon nanotubes is 2 percent.
Placing the carbon nano tube/aluminum mixed powder in a planetary ball mill with a ball-material ratio of 20:1, adding stearic acid with the mass fraction of 1%, performing low-speed ball milling for 7 hours at the rotating speed of 135rpm, and performing high-speed ball milling for 2 hours at the rotating speed of 270rpm to prepare carbon nano tube/aluminum granular composite powder, wherein the scanning electron microscope result of the carbon nano tube/aluminum granular composite powder is shown in figure 4.
Example 2
Nano silicon carbide/aluminum composite powder
Spherical aluminum powder with the average grain size of 400 meshes is adopted, and the purity is more than 99.5 percent; nano silicon carbide particles with the average particle size of 50 nanometers and the weight fraction of nano silicon carbide is 3 percent.
Placing the nano silicon carbide/aluminum mixed powder in a planetary ball mill, wherein the ball-material ratio is 20:1, adding stearic acid with the mass fraction of 1%, and the multistage gradient ball milling process parameters are as follows: r is1＝120rpm，r2＝140rpm，r3＝160rpm，r4＝180rpm，r5＝200rpm，r6＝220rpm，r7＝260rpm，r8＝300rpm；t1＝1h，t2＝1h，t3＝1h，t4＝1h，t5＝1h，t6＝0.5h，t7＝0.5h，t8After the time is 0.5h, the nano silicon carbide/aluminum composite powder is prepared, and the scanning electron microscope result is shown in figure 5.
Example 3
Graphene/copper composite powder
Spherical copper powder with the average particle size of 400 meshes is adopted, the purity is more than 99.5%, graphene nanosheets are 2-5 nanometers in thickness and 1-3 microns in diameter, and the mass fraction of graphene is 1%.
Placing the graphene/copper mixed powder into a stirring type ball mill, adding stearic acid with the mass fraction of 1%, wherein the ball-material ratio is 15:1, and the multi-stage gradient ball milling process parameters are as follows: r is1＝100rpm，r2＝120rpm，r3＝140rpm，r4＝160rpm，r5＝180rpm，r6＝230rpm，r7＝280rpm；t1＝1h，t2＝1h，t3＝1h，t4＝1h，t5＝1h，t6＝1h，t7The scanning electron microscope results of the obtained graphene/copper granular composite powder are shown in fig. 6.
As shown in the figures 1-6, the composite powder obtained by the multistage gradient ball milling method for preparing the nano-phase and the metal powder in a composite mode has the advantages that the nano-phase structure is kept intact and is uniformly dispersed, the nano-phase and the matrix powder are well combined, and the problems of uniform dispersion and interface combination of the nano-phase in the metal powder can be solved. And the energy consumption is saved, the time is saved, the sampling observation is convenient, the optimization and the upgrade of the process are facilitated, and the applicability of the raw materials is widened.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (6)
1. A multistage gradient ball milling method prepared by compounding nano phase and metal powder is characterized by comprising the following steps: performing ball milling on the nano-phase powder and the metal powder at a multi-stage ball milling rotating speed which is gradually increased from low to high to prepare composite powder, and overcoming the processing hardening generated by the ball milling deformation of the metal powder through multi-stage gradient regulation of the ball milling rotating speed;
wherein the ball milling rotating speeds of the multiple stages are n stages, n is an integer larger than or equal to 2, and the ball milling rotating speeds of the first stage to the nth stage are sequentially set as r1～rnSetting the ball milling time corresponding to the ball milling rotation speed of each stage as t1～tn(ii) a The ball milling rotating speed is required to meet the requirementThe parts are as follows: r is not more than 10rpm1～rnR is not less than 1000rpm and not more than 5rpmn-rn-1The speed is less than or equal to 100rpm, and the ball milling time needs to meet the following conditions: t is more than or equal to 0.5h1～tn≤5h。
2. The multistage gradient ball milling method for preparing nanophase and metal powder in composite manner according to claim 1, wherein the nanophase comprises nano carbon nanotubes, carbon nanospheres, carbon nanofibers, carbon nanosheets, carbon nano onions, graphene oxide, redox graphene, nanodiamonds, nano SiC, nano B4C. Nano WC and nano Al2O3Nano ZnO and nano TiO2Nano SiO2Nano ZrO 22Nano AlN, nano TiN and nano TiB2At least one of (1).
3. The multistage gradient ball milling method for preparing nano-phase and metal powder in a composite manner according to claim 1, wherein the metal powder comprises at least one of Al, Cu, Mg, Ti, Fe, Ni, Zn, Zr, Cr, Co and W or alloy powder thereof.
4. The multistage gradient ball milling method prepared by compounding the nano phase and the metal powder according to claim 1, wherein the mass fraction of the nano phase is 0.005-30% of the composite powder.
5. The multistage gradient ball milling method prepared by compounding the nano phase and the metal powder according to claim 1, wherein a material-ball ratio in a ball milling process is 1: 2-100, and a grinding ball diameter is 2-120 mm.
6. The multistage gradient ball milling method for preparing nano-phase and metal powder in a composite manner according to claim 1, wherein a process control agent is added in the ball milling process; the process controller is at least one of methanol, ethanol, titanate, silicone oil, oleic acid, imidazoline, paraffin, cellulose and stearic acid.
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