CN114855126B - A device and method for surface modification of micro-nano powder - Google Patents

Abstract

The invention discloses a device for surface modification of micro-nano powder, which includes a vacuum chamber and a vibrating turning mechanism. The vibrating turning mechanism includes a vibrating bowl and a dust shield. A guide column is installed in the middle of the vibrating bowl. A vibrator and a pillar are installed on the side, and an evaporation source for processing the powder inside the vibrating turning mechanism is installed on the vacuum chamber. The invention also provides a method for surface modification of micro-nano powder, which puts the powder into the vibrating The turning mechanism is modified with an evaporation source. The invention cooperates with the evaporation source through a vibrating turning mechanism to fully expose the surface of each powder to plasma, ensuring a high coating rate of powder surface modification. By combining the vacuum feeding component and the storage component, the invention ensures uniformity Under the premise of the requirements of sex, compactness and purity, the single-time powder processing capacity can reach kilogram level, and surface modification of different micro-nano powders can also be realized. It has broad application prospects and can be used for industrial mass production.

Description

A device and method for surface modification of micro-nano powder

Technical field

The invention belongs to the technical field of surface modification of micro-nano powders, and specifically relates to a device and method for surface modification of micro-nano powders.

Background technique

With people's continuous demand for high-performance materials, various difficulties have been encountered in the research and development of powder metallurgy technology. Among them, the most important technical issue affecting material performance is the interface bonding of materials. In order to solve this problem, researchers have Doping, mechanical alloying and other methods are used to improve interface problems, but these methods have problems such as uneven distribution of elements.

Therefore, in order to obtain excellent interfacial bonding, researchers envision surface modification by coating the powder surface with a core-shell structure of a modified film, and then sintering to improve the interfacial bonding force. However, in order to obtain excellent interfacial bonding, , it is necessary to consider three factors: satisfying the compatibility of interphase thermodynamics, satisfying the coexistence of interphase thermodynamics, and having good wettability between the cladding layer and the core.

As research continues, researchers have discovered that when heterogeneous metal or ceramic powders are combined with metal-based materials, problems such as large differences in solid solubility, mismatch of valence bonds, or incompatibility between metals and ceramics , resulting in the inability to achieve a tight connection between the compounded metal-based material and the compounded powder, and there is a large difference between the experimental value and the theoretically predicted value. The reason is poor wettability, incompatibility with the metal-based material, and inability to effectively compound . The solution is to modify the surface of heterogeneous metal powder or ceramic powder to prepare a modified film that is compatible with metal-based materials to increase wettability and thereby improve interface bonding force.

Powder surface modification technology mainly includes the following methods: chemical plating, chemical vapor deposition, physical deposition, electroplating, plasma method, etc. Among them, plasma method, as a high-quality surface modification method, has also been gradually applied to powder surface modification.

The patent with the publication number CN101798677A discloses a method of surface coating by ultrasonic vibration, the patent with the publication number CN101082120A discloses a method of surface coating with a conical funnel spiral turning, and the patent with the publication number CN103160795A discloses a Drum surface coating method, these three methods all use plasma method to prepare surface-modified powder. On the premise of ensuring uniformity, density, and purity requirements, the amount of powder prepared at one time is small and can only meet the requirements of For micro-amount usage requirements, existing equipment on the market currently prepares around 5g~30g each time, which cannot meet the demand for modified powder in composite material preparation.

Therefore, there is a need for a device and method that can complete the surface modification of a large number of micro-nano powders.

Contents of the invention

The technical problem to be solved by the present invention is to provide a device and method for surface modification of micro-nano powders in view of the above-mentioned deficiencies in the prior art. This device uses a special vibration turning method, combined with a vacuum feeding device and a storage device, to perfectly solve the problem of a small amount of powder processed at a time while ensuring uniformity, density, and purity requirements. , and the powder device can realize the preparation of modified materials such as metals, ceramics and non-metals based on existing equipment and by selecting different evaporation sources.

In order to solve the above technical problems, the technical solution adopted by the present invention is: a device for surface modification of micro-nano powder, which is characterized in that it includes a vacuum chamber, and a vibration turning mechanism is installed in the vacuum chamber. The vibration The material turning mechanism includes a vibrating bowl. The upper part of the vibrating bowl is equipped with a dust shield that opens or closes the vibrating bowl. The middle part of the vibrating bowl is equipped with a guide column. A vibrator is installed on the lower side of the vibrating bowl. A pillar is also installed on the lower side of the bowl to support the vibrating bowl. The vacuum chamber is equipped with an evaporation source for processing the powder inside the vibrating turning mechanism. The lower part of the vibrating bowl is provided with a valve that is opened or closed through a guide column. Material guide port.

The above-mentioned device for modifying the surface of micro-nano powder is characterized in that the evaporation source is a magnetron target source of magnetron sputtering equipment, an arc device or arc source of multi-arc ion plating equipment, gas plasma Electron guns or hollow cathodes of chemical equipment.

The above-mentioned device for modifying the surface of micro-nano powder is characterized in that the bottom of the vibration bowl is spherical, the guide column and the guide port are located at the center of the bottom of the vibration bowl, and the guide column It is in the shape of a truncated cone, and the material guide column and the bottom of the vibrating bowl are connected through a slot; a plurality of vibrating blocks are installed on the outside of the side wall of the vibrating bowl for shedding the powder pasted on the inside of the side wall; the vibrating bowl is connected There is a bias power supply used to negatively charge the powder in the vibrating bowl.

The above-mentioned device for modifying the surface of micro-nano powder is characterized in that the vacuum chamber is connected with a vacuum component for evacuating the vacuum chamber and filling it with protective gas, and the vacuum chamber is provided with a hole for observing vibrations. Bowl viewing window.

The above-mentioned device for surface modification of micro-nano powder is characterized in that a vacuum feeding assembly is installed outside the vacuum chamber, and the vacuum feeding assembly includes a vacuum chamber, a powder chamber and a vibration bowl extending into or out of the Mechanical telescopic tube, the mechanical telescopic tube raises or lowers the guide column.

The above-mentioned device for surface modification of micro-nano powder is characterized in that a material storage component is installed outside the vacuum chamber, and the material storage component includes a material storage chamber and a material storage chamber connected to the material guide port. Feed tube.

In addition, the present invention provides a method for surface modification of micro-nano powder, which is characterized in that the method includes the following steps:

Step 1: Put the powder into the vibrating bowl, close the dust shield, and put the same powder into the vacuum chamber and the powder chamber to obtain a modification device filled with powder;

Step 2: Evacuate the vacuum chamber of the modification device containing the powder obtained in Step 1 and fill it with argon gas, then heat the powder in the vibration bowl, and open the dust shield to obtain the heated Powder modification device;

Step 3: Open the vibrator and vibrating block of the modification device equipped with heated powder obtained in step 2, so that the powder is turned in the vibrating bowl, and at the same time, a bias power supply is loaded on the vibrating bowl to obtain the powder to be modified. body modification device;

Step 4: Open the evaporation source of the modification device containing the powder to be modified obtained in step 3, and modify the powder. After the powder in the vibrating bowl is modified, close the evaporation source and close the dust shield. Move the guide column and put the modified powder into the storage room through the guide pipe to obtain the modified powder and modification device;

Step 5: Send the powder in the vacuum chamber of the modification device obtained in step 4 into the vibrating bowl, send the powder in the powder chamber into the vacuum chamber, and then repeat steps 2 to 4 to clean the powder in the vibrating bowl. The body is modified, and then the powder in the vacuum chamber is sent into the vibration bowl, and steps 2 to 4 are repeated to modify the powder in the vibration bowl, and finally the modified powder is obtained in the storage chamber.

In the present invention, the powder is loaded into the vibrating bowl, the vacuum chamber and the powder chamber respectively, and the powder in the vibrating bowl is first modified. After the powder in the vibrating bowl is modified and output, the powder in the vacuum chamber is The powder is sent to the vibrating bowl for modification and then output. Finally, the powder in the powder chamber is sent to the vibrating bowl for modification and then output. During the modification process, powder can be continuously added to the powder chamber. , continuously carry out powder modification and output without destroying the vacuum conditions in the vacuum chamber, and perform cyclic modification; this method realizes surface modification of various types of powders such as pure metals, alloys, ceramics, etc., and improves the later material properties. research offers endless possibilities.

The above method is characterized in that the mass of the powder described in step one is 1g~2000g. The present invention is not only suitable for modification of a small amount of powder, but also suitable for modification of a large amount of powder, and has a high coating rate, and the coating rate can reach more than 90%.

The above method is characterized in that the pressure in the vacuum chamber in step 2 is 1.0×10 ^-4 Pa~5.0×10 ^-3 Pa, and the heating is to heat the powder to 50°C~400°C. The present invention ensures the modification effect by controlling the pressure in the empty chamber. The purpose of heating the powder in the present invention is to increase the binding force between the powder base material and the plated powder. For different powder base materials, the selected heating temperature varies. Similarly, if the temperature is too high, the powder will easily ignite, and if the temperature is too low, the bonding force will be poor.

The above method is characterized in that the vibration power of the vibrator and the vibration block in step three is 5W~200W, and the voltage output by the bias power supply is 200V~500V. The present invention controls the vibration power of the vibrator and the vibration block to fully mix and modify the powder in the vibrating bowl, thereby ensuring the uniformity of modification and preventing the powder from sticking to the wall of the vibrating bowl; By controlling the voltage output by the bias power supply, the micro-nano powder in the vibrating bowl is negatively charged, attracting and accelerating the plasma generated by the evaporation source, thereby accelerating the deposition speed on the powder surface and enhancing the interaction between the modified film and the powder. Surface adhesion.

Compared with the prior art, the present invention has the following advantages:

1. The present invention provides a vacuum environment for surface modification of micro-nano powder through a vacuum chamber to prevent oxidation of micro-nano powder. Through the vibration turning mechanism, the powder is continuously vibrated in the vibrating bowl, and the powder passes through the vibrator. , making the powder vibrate back and forth from the inside to the outside, vibrating and flipping from the bottom of the vibrating bowl to the side wall, thereby fully exposing and fully modifying the powder surface, ensuring a high coating rate of powder surface modification, through the evaporation source , excite plasma and modify the powder. Depending on the thickness of the modified film, its thickness can be accurately controlled by controlling the time of plasma sputtering and the size of the evaporation source current; a conductor is opened at the bottom of the vibrating bowl. The opening or closing of the material column is used to release the modified powder and facilitate the collection of the powder.

2. The present invention uses a plasma method combined with a vibration turning mechanism to coat the surface of micro-nano powder with a metal, alloy or ceramic film to achieve the purpose of modifying the powder surface and lay the foundation for the preparation of high-performance composite materials. The surface of pure metal/alloy/ceramics and other micro-nano powders and large particle powders is coated with a pure metal/alloy/ceramic modified film layer, which realizes the surface modification of different micro-nano powders and can prepare different types of Modified membranes are divided into metals, ceramics (ceramic phases such as nitrides, oxides, carbides, etc.) and non-metals (graphene, carbon film, silicon film and boron nitride BN) according to the type of modified material film. Realize the preparation process of different modified film thicknesses and multi-layer modified films.

3. The present invention sets up vibrators and vibration blocks to fully expose the surface of each powder to plasma to ensure the uniformity of the modified film. By combining the vacuum feeding component and the material storage component, it meets the needs of industrial production in a single time. The powder processing capacity can reach kilogram level.

4. The method for surface modification of micro-nano powders of the present invention can realize surface modification of various types of powders such as pure metals, alloys, ceramics, etc., providing unlimited possibilities for later research on material properties.

The technical solution of the present invention will be described in further detail below through the drawings and examples.

Description of the drawings

Figure 1 is a schematic structural diagram of the device for surface modification of micro-nano powder according to the present invention.

Figure 2 is a schematic structural diagram of the vacuum chamber of the present invention.

Figure 3 is a schematic structural diagram of the vibrating material turning mechanism of the present invention.

Figure 4 is an SEM image of the modified powder prepared in Example 1 of the present invention.

Explanation of reference symbols:

1—vacuum chamber; 2—vibrating bowl; 3—Dust shield; 4—Guide column; 5—Vibrator; 6—Pillar; 7—Evaporation source; 8—vibrating block; 9—Bias power supply; 10—Vacuum components; 11—Observation window; 12—Vacuum chamber; 13—Powder room; 14—Mechanical telescopic tube; 15—Storage room; 16—Feeding tube.

Detailed ways

A device for surface modification of micro-nano powders of the present invention is described in detail through Example 1.

Example 1

As shown in Figures 1, 2 and 3, the device for surface modification of micro-nano powder in this embodiment includes a vacuum chamber 1. A vibrating turning mechanism is installed in the vacuum chamber 1. The vibrating turning mechanism It includes a vibrating bowl 2. The upper part of the vibrating bowl 2 is equipped with a dust shield 3 that opens or closes the vibrating bowl 2. The middle part of the vibrating bowl 2 is equipped with a guide column 4. A vibrator is installed on the lower side of the vibrating bowl 2. 5. A pillar 6 is also installed on the lower side of the vibrating bowl 2 to support the vibrating bowl 2. An evaporation source 7 is installed on the vacuum chamber 1 to process the powder inside the vibrating turning mechanism. The vibrating bowl 2 The lower part is provided with a material guide port that is opened or closed by the material guide pillar 4.

It should be noted that the vacuum chamber 1 provides a vacuum environment for the surface modification of the micro-nano powder to prevent oxidation of the micro-nano powder, and the vibration turning mechanism causes the powder to continuously vibrate in the vibrating bowl 2, and the powder passes through the vibration The function of the device 5 makes the powder vibrate back and forth from the inside to the outside, vibrate and flip from the bottom of the vibrating bowl 2 to the side wall, thereby fully exposing and fully modifying the powder surface, ensuring high coverage of the powder surface modification. rate, the plasma is excited through the evaporation source 7, and the powder is modified. According to the thickness of the modified film, its thickness can be accurately controlled by controlling the time of plasma sputtering and the current size of the evaporation source 7; by The lower part of the vibrating bowl 2 is provided with a material guide port that is opened or closed by the material guide column 4 for releasing the modified powder to facilitate the collection of the powder.

It should be noted that the support 6 is a spring support 6, the vibrating bowl 2 is supported by the spring support 6, and the spring plays a role of shock absorption.

In this embodiment, the evaporation source 7 is a magnetron target source of magnetron sputtering equipment, an arc device or arc source of multi-arc ion plating equipment, an electron gun or a hollow cathode of gas plasma equipment. By using different evaporation sources 7, it is suitable for different powders to be modified.

As shown in Figures 1 and 3, in this embodiment, the bottom of the vibrating bowl 2 is spherical, the guide post 4 and the guide opening are located at the center of the bottom of the vibrating bowl 2, and the guide post 4 is truncated. , the guide column 4 and the bottom of the vibrating bowl 2 are connected through a slot; a plurality of vibrating blocks 8 are installed on the outside of the side wall of the vibrating bowl 2 for shedding the powder pasted on the inside of the side wall; the vibrating bowl 2 is connected to a bias power supply 9 for negatively charging the powder in the vibrating bowl 2 . The bottom of the vibrating bowl 2 is spherical, and the guide post 4 and the guide port are located at the center of the bottom of the vibrating bowl 2, so that the powder in the vibrating bowl 2 is concentrated toward the center of the bottom of the vibrating bowl 2 under the action of vibration, and passes through the guide. The material column 4 rolls, and the powder moves in the direction of the arrow in Figure 3. When the powder is collected after the modification is completed, the spherical bottom also facilitates the centralized collection of powder. The guide column 4 and the bottom of the vibration bowl 2 are connected through a slot. To ensure that the two are tightly connected and the powder will not leak during the modification process, the guide column 4 is lifted or lowered through the mechanical telescopic tube 14 of the vacuum feeding assembly to control the release of modified powder in the vibration bowl 2. By adjusting the vibration motor Vibration frequency, the surface of the kilogram-level micro-nano powder in the vibration bowl 2 is continuously exposed to the plasma substance, so that it has almost the same exposure time, so that the surface of the micro-nano powder is coated with the same and uniform modification thickness membrane, the vibrating blocks 8 on the side wall of the vibrating bowl 2, there is no clear requirement for the number of vibrating blocks 8, it can be increased according to the degree of stickiness of the powder on the side wall, and the size can be changed according to actual needs. The vibration causes the powder to stick to the side wall. The particles fall off, thereby ensuring a high coating rate of powder surface modification; the micro-nano powder in the vibrating bowl 2 is negatively charged through the bias power supply 9, and the plasma generated by the evaporation source 7, such as metal cations or non-metal cations, is generated Attraction and acceleration, thereby speeding up the deposition speed on the powder surface, enhancing the binding force between the modified film and the powder surface, and improving the modification efficiency.

As shown in Figure 1, in this embodiment, the vacuum chamber 1 is connected to a vacuum assembly 10 for evacuating the vacuum chamber 1 and filling it with protective gas. The vacuum chamber 1 is provided with an observation window 11 for observing the vibrating bowl 2. . Through the observation window 11, observe the vibration state of the powder to adjust the vibration power of the vibration motor.

As shown in Figures 1 and 3, in this embodiment, a vacuum feeding assembly is installed outside the vacuum cabin 1. The vacuum feeding assembly includes a vacuum chamber 12, a powder chamber 13 and a mechanical telescopic tube extending into or out of the vibrating bowl 2. 14. The mechanical telescopic tube 14 raises or lowers the guide column 4. By setting up the vacuum chamber 12 and the powder chamber 13, the powder therein is transported to the vibrating bowl 2 in a circular cycle. During the modification process, powder can be continuously added to the powder chamber 13 without destroying the vacuum chamber 1. Continuously carry out powder modification and output under vacuum conditions, and perform cyclic modification. The powder in the vacuum chamber 12 is put into the vibrating bowl 2 by setting a mechanical telescopic tube 14, and the powder to be surface modified is placed separately. Enter the vacuum chamber 12 and the powder chamber 13. After the surface modification of the powder in the vibrating bowl 2 is completed, it is introduced into the storage assembly, and the micro-nano powder in the vacuum chamber 12 is introduced into the vibrating bowl 2 through the mechanical telescopic tube 14. , and then introduce the powder in the powder chamber 13 into the vacuum chamber 12 and evacuate it to prepare for continuous production. When adding powder to the vibrating bowl 2, there is no need to destroy the vacuum environment and it will not affect the surface modification, and continuous production can be carried out. Surface modification.

It should be noted that there is a gap of 2cm~3cm between the vibration bowl 2 and the dust shield 3. When the dust shield 3 is closed, the guide post is lifted from the slot through the guide tube 16, and the powder enters the guide tube. 16. The tubes and slots in this equipment are telescopically designed to increase the controllability of the device.

As shown in FIG. 1 , in this embodiment, a material storage assembly is installed outside the vacuum chamber 1 . The material storage assembly includes a material storage chamber 15 and a material guide pipe 16 connecting the material storage chamber 15 and the material guide port. The modified powder is introduced into the storage assembly through the feed tube 16, and the powder is vacuum packed through the storage assembly to avoid contamination. After the powder in the vibrating bowl 2 has been modified, remove the guide column 4 in the vibrating bowl 2, and the modified powder enters the storage chamber 15 through the guide tube 16. The storage chamber 15 has a built-in vacuum sealing machine. The powder enters the vacuum packaging bag and is vacuum packed to better avoid oxidation contamination of the powder.

A method for surface modification of micro-nano powders of the present invention is described in detail through Examples 2 to 4.

Example 2

This embodiment includes the following steps:

Step 1: Divide the powder into three equal parts and put them into the vibration bowl 2, the vacuum chamber 12 and the powder chamber 13 respectively, close the dust shield 3, and obtain a modification device filled with powder; the powder is the total amount 150g, Ti powder with particle size 50nm~100nm;

Step 2: Evacuate the vacuum chamber 1 of the modification device containing the powder obtained in step 1 and fill it with argon gas, then heat the powder in the vibration bowl 2 and open the dust shield 3 to obtain Equipped with a modification device for heating the powder; the pressure in the vacuum chamber 1 is 1.0×10 ^-4 Pa, and the heating is to heat the powder to 120°C;

Step 3: Open the vibrator 5 and the vibrating block 8 equipped with the modification device for heating the powder obtained in the step 2, so that the powder is turned over in the vibrating bowl 2, and at the same time, the bias power supply 9 is loaded on the vibrating bowl 2 to obtain A modification device is equipped with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 5W~100W, and the voltage output by the bias power supply 9 is 200V;

Step 4: Open the evaporation source 7 of the modification device containing the powder to be modified obtained in step 3 to modify the powder. After the powder in the vibrating bowl 2 is modified, close the evaporation source 7 and close the barrier. Dust plate 3 moves the material guide column 4, and the modified powder enters the material storage chamber 15 through the material guide tube 16 to obtain the modified powder and modification device; the evaporation source 7 is three magnetron sputtering power supplies, Equipped with a DC power supply and using high-purity Cu metal target material to excite Cu ions, and adjust the angles of the three magnetron targets to maximize the sputtering area of Cu ions in the vibrating bowl 2;

Step 5: Send the powder in the vacuum chamber 12 of the modification device obtained in step 4 into the vibrating bowl 2, send the powder in the powder chamber 13 into the vacuum chamber 12, and then repeat steps 2 to 4. The powder in the vibrating bowl 2 is modified, and then the powder in the vacuum chamber 12 is sent into the vibrating bowl 2. Repeat steps two to four to modify the powder in the vibrating bowl 2, and finally in the storage chamber 15 Modified powder was obtained.

After testing, the modified powder prepared in this example prepares a metallic Cu layer on the surface of Ti powder, with a coating rate of more than 92%. The modified powder can prepare Ti alloy composite reinforced materials, significantly improving the strength and plasticity. .

Figure 4 is an SEM image of the modified powder prepared in this embodiment. It can be seen from Figure 4 that the surface of the Ti powder is coated with an obvious Cu layer, and the coating is uniform and continuous, which can achieve the purpose of surface modification of the titanium powder.

Example 3

This embodiment includes the following steps:

Step 1: Put the powder into the vibrating bowl 2, close the dust shield 3, and obtain a modification device filled with powder; the powder is 500g Al ₂ O ₃ powder with a particle size of 200 μm ~ 300 μm;

Step 2: Evacuate the vacuum chamber 1 of the modification device containing the powder obtained in step 1 and fill it with argon gas, then heat the powder in the vibration bowl 2 and open the dust shield 3 to obtain Equipped with a modification device for heating the powder; the pressure in the vacuum chamber 1 is 2.0×10 ^-3 Pa, and the heating is to heat the powder to 100°C;

Step 3: Open the vibrator 5 and the vibrating block 8 equipped with the modification device for heating the powder obtained in the step 2, so that the powder is turned over in the vibrating bowl 2, and at the same time, the bias power supply 9 is loaded on the vibrating bowl 2 to obtain A modification device is equipped with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 50W~100W, and the voltage output by the bias power supply 9 is 200V;

Step 4: Open the evaporation source 7 of the modification device containing the powder to be modified obtained in step 3 to modify the powder. After the powder in the vibrating bowl 2 is modified, close the evaporation source 7 and close the barrier. Dust plate 3 moves the material guide column 4, and the modified powder enters the material storage chamber 15 through the material guide tube 16, and the modified powder is obtained in the material storage chamber 15; the evaporation sources 7 are three, respectively, to excite Cu , Zr and Cr magnetron sputtering power supply.

After testing, the modified powder prepared in this example is to prepare metal Cu, Zr, and Cr layers on the surface of Al ₂ O ₃ powder, with a coating rate of more than 93%. The modified powder is a good alloy reinforcement phase. , especially in high-entropy alloys, which has a significant reinforcing effect.

Real case 4

This embodiment includes the following steps:

Step 1: Divide the powder into three equal parts and put them into the vibration bowl 2, the vacuum chamber 12 and the powder chamber 13 respectively, close the dust shield 3, and obtain a modification device filled with powder; the powder is the total amount 500g Ni ₃ Al powder with particle size 0.5mm~1mm;

Step 2: Evacuate the vacuum chamber 1 of the modification device containing the powder obtained in step 1 and fill it with argon gas, then heat the powder in the vibration bowl 2 and open the dust shield 3 to obtain Equipped with a modification device for heating the powder; the pressure in the vacuum chamber 1 is 2.0×10 ^-3 Pa, and the heating is to heat the powder to 200°C;

Step 3: Open the vibrator 5 and the vibration block 8 of the modification device equipped with heated powder obtained in step 2, so that the powder is turned over in the vibrating bowl 2 to obtain a modification device equipped with the powder to be modified; The vibration power of the vibrator 5 and the vibration block 8 is 100W~200W;

Step 4: Open the evaporation source 7 of the modification device containing the powder to be modified obtained in step 3 to modify the powder. After the powder in the vibrating bowl 2 is modified, close the evaporation source 7 and close the barrier. The dust plate 3 moves the material guide column 4, and the modified powder enters the material storage chamber 15 through the material guide tube 16 to obtain the modified powder and the modification device; the evaporation source 7 is a gas plasma generation source and is equipped with According to the power supply, argon gas is introduced into the gas plasma generation source as the hot electron excitation gas, and acetylene gas is filled into the hot electron outlet to crack the acetylene gas into carbon ions and hydrogen ions, and the carbon ions are deposited into the Ni ₃ Al powder. On the surface, graphene Gr forms SP3 bonds. Due to the presence of hydrogen ions, what is obtained here is not pure graphene Gr;

Step 5: Send the powder in the vacuum chamber 12 of the modification device obtained in step 4 into the vibrating bowl 2, send the powder in the powder chamber 13 into the vacuum chamber 12, and then repeat steps 2 to 4. The powder in the vibrating bowl 2 is modified, and then the powder in the vacuum chamber 12 is sent into the vibrating bowl 2. Repeat steps two to four to modify the powder in the vibrating bowl 2, and finally in the storage chamber 15 Modified powder was obtained.

After testing, the modified powder prepared in this example is a graphene layer prepared on the surface of Ni ₃ Al powder, with a coating rate of more than 93%. Due to its high strength, graphene has been used in the preparation of high-strength alloys. Widely concerned, coating graphene on the powder surface in this way fundamentally solves the problem of uneven distribution of graphene in powder metallurgy.

Example 5

This embodiment includes the following steps:

Step 1: Divide the powder into three equal parts and put them into the vibration bowl 2, the vacuum chamber 12 and the powder chamber 13 respectively, close the dust shield 3, and obtain a modification device filled with powder; the powder is the total amount 2000g, Ti powder with particle size 200nm~500nm;

Step 2: Evacuate the vacuum chamber 1 of the modification device containing the powder obtained in step 1 and fill it with argon gas, then heat the powder in the vibration bowl 2 and open the dust shield 3 to obtain Equipped with a modification device for heating the powder; the pressure in the vacuum chamber 1 is 5.0×10 ^-3 Pa, and the heating is to heat the powder to 400°C;

Step 3: Open the vibrator 5 and the vibrating block 8 equipped with the modification device for heating the powder obtained in the step 2, so that the powder is turned over in the vibrating bowl 2, and at the same time, the bias power supply 9 is loaded on the vibrating bowl 2 to obtain A modification device equipped with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 150W~200W, and the voltage output by the bias power supply 9 is 50V;

Step 4: Open the evaporation source 7 of the modification device containing the powder to be modified obtained in step 3 to modify the powder. After the powder in the vibrating bowl 2 is modified, close the evaporation source 7 and close the barrier. Dust plate 3 moves the material guide column 4, and the modified powder enters the material storage chamber 15 through the material guide tube 16 to obtain the modified powder and modification device; the evaporation source 7 is three magnetron sputtering power supplies, Equipped with a DC power supply and using high-purity Cu metal target material to excite Cu ions, and adjust the angles of the three magnetron targets to maximize the sputtering area of Cu ions in the vibrating bowl 2;

Step 5: Send the powder in the vacuum chamber 12 of the modification device obtained in step 4 into the vibrating bowl 2, send the powder in the powder chamber 13 into the vacuum chamber 12, and then repeat steps 2 to 4. The powder in the vibrating bowl 2 is modified, and then the powder in the vacuum chamber 12 is sent into the vibrating bowl 2. Repeat steps two to four to modify the powder in the vibrating bowl 2, and finally in the storage chamber 15 Modified powder was obtained.

After testing, the modified powder prepared in this example prepares a metallic Cu layer on the surface of Ti powder, with a coating rate of more than 92%. The modified powder can prepare Ti alloy composite reinforced materials, significantly improving the strength and plasticity. .

Example 6

This embodiment includes the following steps:

Step 1: Divide the powder into three equal parts and put them into the vibration bowl 2, the vacuum chamber 12 and the powder chamber 13 respectively, close the dust shield 3, and obtain a modification device filled with powder; the powder is the total amount 1500g Ti powder with particle size 500μm~800μm;

Step 2: Evacuate the vacuum chamber 1 of the modification device containing the powder obtained in step 1 and fill it with argon gas, then heat the powder in the vibration bowl 2 and open the dust shield 3 to obtain Equipped with a modification device for heating the powder; the pressure in the vacuum chamber 1 is 1.0×10 ^-4 Pa, and the heating is to heat the powder to 50°C;

Step 3: Open the vibrator 5 and the vibrating block 8 equipped with the modification device for heating the powder obtained in the step 2, so that the powder is turned over in the vibrating bowl 2, and at the same time, the bias power supply 9 is loaded on the vibrating bowl 2 to obtain A modification device is equipped with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 180W~200W, and the voltage output by the bias power supply 9 is 100V;

Step 4: Open the evaporation source 7 of the modification device containing the powder to be modified obtained in step 3 to modify the powder. After the powder in the vibrating bowl 2 is modified, close the evaporation source 7 and close the barrier. Dust plate 3 moves the material guide column 4, and the modified powder enters the material storage chamber 15 through the material guide tube 16 to obtain the modified powder and modification device; the evaporation source 7 is three magnetron sputtering power supplies, Equipped with a DC power supply and using high-purity Cu metal target material to excite Cu ions, and adjust the angles of the three magnetron targets to maximize the sputtering area of Cu ions in the vibrating bowl 2;

Step 5: Send the powder in the vacuum chamber 12 of the modification device obtained in step 4 into the vibrating bowl 2, send the powder in the powder chamber 13 into the vacuum chamber 12, and then repeat steps 2 to 4. The powder in the vibrating bowl 2 is modified, and then the powder in the vacuum chamber 12 is sent into the vibrating bowl 2. Repeat steps two to four to modify the powder in the vibrating bowl 2, and finally in the storage chamber 15 Modified powder was obtained.

After testing, the modified powder prepared in this example prepares a metallic Cu layer on the surface of Ti powder, with a coating rate of more than 91%. The modified powder can prepare Ti alloy composite reinforced materials, significantly improving the strength and plasticity. .

The above descriptions are only preferred embodiments of the present invention and do not limit the present invention in any way. Any simple modifications, changes and equivalent changes made to the above embodiments based on the technical essence of the invention still fall within the protection scope of the technical solution of the invention.

Claims (9)

1. A device for surface modification of micro-nano powder, characterized in that it includes a vacuum chamber (1), a vibrating turning mechanism is installed in the vacuum chamber (1), and the vibrating turning mechanism includes a vibrating bowl (2), the upper part of the vibration bowl (2) is equipped with a dust shield (3) that opens or closes the vibration bowl (2), and the middle part of the vibration bowl (2) is equipped with a guide column (4). A vibrator (5) is installed on the lower side of the vibration bowl (2). A pillar (6) is also installed on the lower side of the vibration bowl (2) to support the vibration bowl (2). A vibrator (5) is installed on the vacuum chamber (1). There is an evaporation source (7) for processing the powder inside the vibrating turning mechanism. The lower part of the vibrating bowl (2) is provided with a material guide port that is opened or closed by the material guide column (4). The vibrating bowl (2) The bottom is spherical, and the material guide column (4) and the material guide port are located at the center of the bottom of the vibrating bowl (2). The material guide column (4) is truncated, and the material guide column (4) and the vibration The bottom of the bowl (2) is connected through a slot; a plurality of vibration blocks (8) are installed on the outside of the side wall of the vibrating bowl (2) for shedding the powder stuck on the inside of the side wall; the vibrating bowl (2) A bias power supply (9) for negatively charging the powder in the vibrating bowl (2) is connected. 2. A device for surface modification of micro-nano powder according to claim 1, characterized in that the evaporation source (7) is a magnetron target source of magnetron sputtering equipment or a multi-arc ion plating equipment. Arc device or arc source, electron gun or hollow cathode of gas plasma equipment. 3. A device for surface modification of micro-nano powder according to claim 1, characterized in that the vacuum chamber (1) is connected with a device for evacuating the vacuum chamber (1) and filling it with protective gas. Vacuum assembly (10), the vacuum chamber (1) is provided with an observation window (11) for observing the vibration bowl (2). 4. A device for surface modification of micro-nano powder according to claim 1, characterized in that a vacuum feeding assembly is installed outside the vacuum chamber (1), and the vacuum feeding assembly includes a vacuum chamber (12 ), a powder chamber (13) and a mechanical telescopic tube (14) extending into or out of the vibrating bowl (2). The mechanical telescopic tube (14) raises or lowers the guide column (4). 5. A device for surface modification of micro-nano powder according to claim 1, characterized in that a material storage component is installed outside the vacuum chamber (1), and the material storage component includes a material storage chamber ( 15) and the material guide pipe (16) connecting the material storage chamber (15) and the material guide port. 6. A method for surface modification of micro-nano powder using the device according to any one of claims 1 to 5, characterized in that the method includes the following steps: Step 1. Put the powder into the vibrating bowl (2), close the dust shield (3), and put the same powder into the vacuum chamber (12) and the powder chamber (13) to obtain a container filled with powder. modification device; Step 2: Evacuate the vacuum chamber (1) of the modification device containing the powder obtained in step 1 and fill it with argon gas. Then heat the powder in the vibration bowl (2) and open the dust barrier. Plate (3) to obtain a modification device equipped with heated powder; Step 3: Open the vibrator (5) and the vibration block (8) equipped with the modification device for heating the powder obtained in step 2, so that the powder is turned in the vibrating bowl (2), and at the same time, the vibrating bowl (2) is ) Load the bias power supply (9) to obtain a modification device containing the powder to be modified; Step 4: Open the evaporation source (7) of the modification device containing the powder to be modified obtained in step 3, modify the powder, and close the evaporation source after the powder in the vibrating bowl (2) is modified. (7), close the dust shield (3), move the guide column (4), and enter the modified powder into the storage chamber (15) through the guide pipe (16) to obtain the modified powder and modification device; Step 5: Send the powder in the vacuum chamber (12) of the modification device obtained in step 4 into the vibrating bowl (2), send the powder in the powder chamber (13) into the vacuum chamber (12), and then Repeat steps two to four to modify the powder in the vibrating bowl (2), and then send the powder in the vacuum chamber (12) into the vibrating bowl (2). Repeat steps two to four to modify the vibrating bowl (2). 2) The internal powder is modified, and finally the modified powder is obtained in the storage chamber (15). 7. The method according to claim 6, characterized in that the mass of the powder in step one is 1g to 2000g. 8. The method according to claim 6, characterized in that the pressure in the vacuum chamber (1) in step 2 is 1.0×10 ^-4 Pa ~ 5.0×10 ^-3 Pa, and the heating is to convert the powder into Heat to 50℃~400℃. 9. The method according to claim 6, characterized in that the vibration power of the vibrator (5) and the vibration block (8) in step three is 5W ~ 200W, and the voltage output by the bias power supply (9) It is 200V~500V.