CN112453417A - Method for preparing Ho-Al nano-scale alloy particles by direct current arc method - Google Patents
Method for preparing Ho-Al nano-scale alloy particles by direct current arc method Download PDFInfo
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- CN112453417A CN112453417A CN202011414893.6A CN202011414893A CN112453417A CN 112453417 A CN112453417 A CN 112453417A CN 202011414893 A CN202011414893 A CN 202011414893A CN 112453417 A CN112453417 A CN 112453417A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C22C21/00—Alloys based on aluminium
Abstract
A method for preparing Ho-Al nano-scale alloy particles by a direct current arc method belongs to the field of preparation of nano-scale magnetic materials. The method comprises the following steps: mixing pure Ho and pure Al according to a weight ratio of 1: 1-1: 3, and smelting the mixture into an alloy block by using a direct current arc under argon; the method comprises the steps of placing bulk HoAl alloy to be evaporated in a plasma arc furnace, flushing hydrogen-helium mixed gas, working the arc, and circularly passivating by using argon. The method can effectively control the size and the appearance of the Ho-Al nano alloy particles by adjusting the current and the voltage, and is a simple method for preparing the Ho-Al nano alloy particles with strong controllability. The method adopts a conventional physical method to prepare required tools, has the advantages of large temperature gradient, easy generation of difficult-to-form alloy structure and capability of providing a good sample for mechanism research.
Description
Technical Field
The invention relates to the field of preparation of nano-scale magnetic materials, in particular to a method for preparing Ho-Al nano-scale alloy particles by using a direct current arc method.
Background
Ho and Al micron-sized particles are widely concerned as reinforcing and modifying components of sintered neodymium iron boron materials. The Ho and Al micron-sized particles can improve the density, corrosion resistance, magnetic performance and use temperature range of the sintered neodymium iron boron material. However, the rare earth elements Ho and the transition metal Al are added to affect the performance of the alloy, and the use is limited. In order to reduce the using amount of non-magnetic materials and rare earth materials, Ho and Al nano-scale particles are adopted to solve the problems. The nanometer level powder is in a highly activated state due to the special volume and surface effect, is particularly sensitive to the environment and is easy to generate chemical action with gas and liquid molecules in the environment, so that the surfaces of Ho and Al nanometer level particles exposed in the air are extremely easy to oxidize and spontaneously combust. Therefore, it is required to prepare Ho-Al nano-scale alloy particles which are relatively stable in air and have excellent performance.
With the development of scientific technology, the research on the performance, structure, preparation and application of nano materials has become a hotspot in the materials science in the world nowadays. The existing preparation methods of the nano-particles comprise a mechanical method, a physical method and a chemical method, wherein the nano-particles prepared by the physical method have high purity and high activity. Arc plasma is an effective method for forming specific nanostructures because it can produce extremely high non-equilibrium states. However, for composite metal nanoparticles (i.e. coating metal particles with other materials), mass production by arc plasma method is still impossible.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing Ho-Al nano-scale alloy particles by using a direct current arc method.
The technical scheme adopted by the invention is as follows: a method for preparing Ho-Al nano-scale alloy particles by a direct current arc method is technically characterized by comprising the following steps of,
step 1, mixing pure Ho and pure Al according to a weight ratio of 1: 1-1: 3, smelting the mixture into an alloy block by using a direct current arc under argon, performing vacuum heat treatment at 400-600 ℃ for 6-15 h, placing the block HoAl alloy to be evaporated on a copper anode target in a plasma arc furnace, and taking a tungsten rod as a cathode; pumping the working chamber to a pressure of 1 × 10-3Pa～2×10-3An environment of Pa;
Step 3, starting circulating water and a power supply to enable the electric arc working current to be 120-180A, the voltage to be 30-50V and the arc striking time to be 0.5-1 h;
step 4, use 5X 10 after stopping the arc3～6×103Air and 9.4X 104～9.5×104Circularly passivating the mixed gas of argon for 18-25 h to prepare Ho2Al17Nanoscale alloy particles.
In the scheme, the diameter of the tungsten rod is 4-6 mm, and the length of the tungsten rod is 150 mm.
In the scheme, the purity of the argon is 99.99%; the purity of the hydrogen gas is 99.95%; the purity of the helium gas was 99.999%.
The method for preparing Ho-Al nano-scale alloy particles by direct current arc process according to claim 1, wherein the prepared Ho2Al1793 percent of nano-scale alloy particles, and the prepared Ho2Al17The distribution of the nano-scale alloy particles is 18-73 nm, and the average particle size is 56-71 nm.
The invention has the beneficial effects that: the method for preparing the Ho-Al nano-scale alloy particles by using the direct current arc method comprises the following steps: mixing pure Ho and pure Al according to a weight ratio of 1: 1-1: 3, and smelting the mixture into an alloy block by using a direct current arc under argon; the method comprises the steps of placing bulk HoAl alloy to be evaporated in a plasma arc furnace, flushing hydrogen-helium mixed gas, working the arc, and circularly passivating by using argon. The method can effectively control the size and the appearance of the Ho-Al nano alloy particles by adjusting the current and the voltage, and is a simple method for preparing the Ho-Al nano alloy particles with strong controllability. The method adopts a conventional physical method to prepare required tools, has the advantages of large temperature gradient, easy generation of difficult-to-form alloy structure and capability of providing a good sample for mechanism research.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is an x-ray diffraction spectrum of a Ho-Al composite nano alloy powder according to an embodiment of the present invention;
FIG. 2 is a typical morphology of Ho-Al nano-scale alloy particles observed by a scanning electron microscope in an embodiment of the present invention;
FIG. 3 is a transmission electron microscope image of an embodiment of the present invention.
Detailed Description
The above objects, features and advantages of the present invention will become more apparent from the following detailed description of the present invention with reference to the accompanying drawings 1 to 3.
Example 1:
the method for preparing Ho-Al nano-scale alloy particles by using the direct current arc method adopted by the embodiment comprises the following steps:
step 1, mixing pure Ho and pure Al according to a weight ratio of 1:1, smelting the mixture into an alloy block by using a direct current arc under argon with the purity of 99.99 percent, and carrying out vacuum heat treatment for 8 hours at 500 ℃. The block HoAl alloy to be evaporated is placed on a copper anode target in a plasma arc furnace, a tungsten rod is used as a cathode, and the diameter (phi) of a black rod is 4mm and the length of the black rod is 150 mm. Pumping the working chamber to 2 × 10-3An environment of Pa;
Step 3, starting circulating water and a power supply to enable the arc current to be 120A, the voltage to be 30V and the arc striking time to be 1 h;
step 4, use 5X 10 after stopping the arc3Air and 9.5X 104The mixed gas of argon is circularly passivated for 20 hours to prepare Ho2Al17Nanoscale alloy particles.
For Ho by using the method of the embodiment2Al17When the nano-scale alloy particles are adjusted, if the current and the voltage are adjusted to be large, the nano-particles with larger particles and wider particle size distribution can be prepared. When the hydrogen content ratio in the mixed gas is increased, the average particle diameter of the nanoparticles is increased, but the anode block is liable to crack, which affects continuous production. If the flow speed of the working gas is adjusted quickly, the particle size distribution of the nanoparticles is narrow. When the temperature and velocity of the working gas are adjusted, the velocity increases as the temperature decreases. When the arc current is increased to about 200A and the working voltage is higher than 40V, the new nano alloy particles can be prepared.
Example 2:
step 1, mixing pure Ho and pure Al according to a weight ratio of 1:3, smelting the mixture into an alloy block by using a direct current arc under argon with the purity of 99.99 percent, and carrying out vacuum heat treatment for 12 hours at the temperature of 600 ℃; the block to be evaporated is placed on a copper anode target, a tungsten rod is used as a cathode, and the diameter (phi) of the black rod is 5mm and the length of the black rod is 150 mm. (ii) a Pumping the working chamber to a pressure of 1 × 10-3Environment of Pa.
Step 3, starting circulating water and a power supply to enable the arc current to be 150A, the voltage to be 30V and the arc striking time to be 0.5 h;
step 4, use 5X 10 after stopping the arc3Air and 9.5X 104The mixed gas of argon is circularly passivated for 24 hours to prepare Ho2Al17Nanoscale alloy particles.
Example 3:
step 1, mixing pure Ho and pure Al according to the weight ratio of 1:2, and smelting the mixture into a compound by using direct current electric arc under the condition of argon with the purity of 99.99 percentCarrying out vacuum heat treatment on the gold block body at 400 ℃ for 15 h; the block to be evaporated is placed on a copper anode target, a tungsten rod is used as a cathode, and the diameter (phi) of the black rod is 6mm and the length is 150 mm. Pumping the working chamber to a pressure of 1 × 10-3Environment of Pa.
Step 3, starting circulating water and a power supply to enable the arc current to be 180A, the voltage to be 50V and the arc striking time to be 1 h;
step 4, use 6X 10 after stopping the arc3Air and 9.4X 104The mixed gas of argon is circularly passivated for 18h to prepare Ho2Al17Nanoscale alloy particles.
It can be confirmed from the X-ray diffraction chart of FIG. 1 that the test sample is Ho2Al17Nanoscale alloy particles.
From the scanning electron micrograph of fig. 2, it can be confirmed that the test sample is a nanoparticle having a spherical-like shape with an average particle diameter of 81 nm.
From the transmission electron microscopy images and the energy spectrum images of fig. 3, the main image is a high-resolution photograph, and the upper right-hand image is an energy spectrum image photographed in the black frame region of the main image, and indicates the nano-alloy (Ho-Al) particles having the amorphous oxide layer. The particles were about 18nm with an outer layer of about 2 nm. The interlayer spacing is judged to be Ho2Al17. It can be demonstrated that the test sample is a nanoparticle, quasi-spherical, with a particle coating;
the above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (4)
1. A method for preparing Ho-Al nano-scale alloy particles by a direct current arc method is characterized by comprising the following steps,
step 1, mixing pure Ho and pure Al according to a weight ratio of 1: 1-1: 3, smelting the mixture into an alloy block by using a direct current arc under argon, performing vacuum heat treatment at 400-600 ℃ for 6-15 h, placing the block HoAl alloy to be evaporated on a copper anode target in a plasma arc furnace, and taking a tungsten rod as a cathode; pumping the working chamber to a pressure of 1 × 10-3Pa～2×10-3An environment of Pa;
step 2, the working chamber is flushed twice with argon gas, and then filled with argon gas with total pressure of 0.95 multiplied by 105Pa hydrogen-helium mixed gas with pressure ratio of helium gas to hydrogen gas being PHe;PH2=2:1 to 9: 1; or total pressure of 0.95X 105Pa hydrogen-argon mixed gas, wherein the pressure ratio of the argon gas to the hydrogen gas is PAr;PH2=2:1~7:1；
Step 3, starting circulating water and a power supply to enable the electric arc working current to be 120-180A, the voltage to be 30-50V and the arc striking time to be 0.5-1 h;
step 4, use 5X 10 after stopping the arc3～6×103Air and 9.4X 104～9.5×104Circularly passivating the mixed gas of argon for 18-25 h to prepare Ho2Al17Nanoscale alloy particles.
2. The method for preparing Ho-Al nano-scale alloy particles by using the direct current arc method according to claim 1, wherein the tungsten rod has a diameter of 4-6 mm and a length of 150 mm.
3. The method for preparing Ho-Al nano-sized alloy particles by the direct current arc method according to claim 1, wherein the purity of the argon gas is 99.99%; the purity of the hydrogen gas is 99.95%; the purity of the helium gas was 99.999%.
4. The method for preparing Ho-Al nano-scale alloy particles by direct current arc process according to claim 1, wherein the prepared Ho2Al1793 percent of nano-scale alloy particles, and the prepared Ho2Al17The distribution of the nano-scale alloy particles is 18-73 nm, and the average particle size is 56-71 nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115582551A (en) * | 2021-07-05 | 2023-01-10 | 无锡金鹏环保科技有限公司 | Process for continuously preparing nano metal powder in liquid phase environment |
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Patent Citations (9)
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| US4981532A (en) * | 1987-08-19 | 1991-01-01 | Mitsubishi Kinzoku Kabushiki Kaisha | Rare earth-iron-boron magnet powder and process of producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115582551A (en) * | 2021-07-05 | 2023-01-10 | 无锡金鹏环保科技有限公司 | Process for continuously preparing nano metal powder in liquid phase environment |
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