CN114855126B - Device and method for modifying surface of micro-nano powder - Google Patents
Device and method for modifying surface of micro-nano powder Download PDFInfo
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- CN114855126B CN114855126B CN202210618223.9A CN202210618223A CN114855126B CN 114855126 B CN114855126 B CN 114855126B CN 202210618223 A CN202210618223 A CN 202210618223A CN 114855126 B CN114855126 B CN 114855126B
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention discloses a device for modifying the surface of micro-nano powder, which comprises a vacuum cabin and a vibration stirring mechanism, wherein the vibration stirring mechanism comprises a vibration bowl and a dust baffle plate, a material guide column is arranged in the middle of the vibration bowl, a vibrator and a support column are arranged at the lower side of the vibration bowl, an evaporation source for processing the powder in the vibration stirring mechanism is arranged on the vacuum cabin, and the invention also provides a method for modifying the surface of the micro-nano powder. According to the invention, the vibration stirring mechanism is matched with the evaporation source, so that the surface of each powder is fully exposed to plasma, the high coating rate of powder surface modification is ensured, and the single powder treatment capacity can reach the kilogram level on the premise of ensuring the uniformity, compactness and purity by combining the vacuum feeding component and the storage component, and the surface modification of different micro-nano powder is realized, so that the method has a wide application prospect and can be used for industrialized mass production.
Description
Technical Field
The invention belongs to the technical field of micro-nano powder surface modification, and particularly relates to a device and a method for modifying the surface of micro-nano powder.
Background
With the continuous demand of high-performance materials, various difficulties are encountered in the research and development of powder metallurgy technology, wherein the most important technical problem affecting the material performance is interface combination of materials, and in order to solve the problem, researchers improve interface problems by doping, mechanical alloying and other methods, but the methods have the problems of uneven element distribution and the like.
Therefore, in order to obtain excellent interfacial bonding, researchers have conceived to improve interfacial bonding by surface modification by a method of coating a core-shell structure of a modified film on a powder surface, followed by sintering, but to obtain excellent interfacial bonding, factors of satisfying compatibility of interphase thermodynamics, satisfying coexistence of interphase thermodynamics, and good wettability between a clad layer and a core must be considered.
With the continuous development of research, researchers find that when heterogeneous metal or ceramic powder is compounded with metal-based materials, the problems of large solid solubility difference, mismatching of valence bonds, incompatibility of metal and ceramic and the like cause that the connection between the compounded metal-based materials and the compounded powder cannot achieve a tight effect, and the experimental value and the theoretical predicted value have large difference, because of poor wettability, the incompatibility with the metal-based materials and the incapability of effective compounding. The solution is to prepare a modified film compatible with metal base materials by modifying the surface of heterogeneous metal powder or ceramic powder, so as to increase wettability and further improve interface binding force.
The powder surface modifying technology mainly includes the following methods, such as chemical plating, chemical vapor deposition, physical deposition, electroplating, plasma method, etc. Among them, the plasma method is also gradually applied to powder surface modification as a high-quality surface modification method.
The patent with publication No. CN101798677A discloses a method for coating a film on a surface by ultrasonic vibration, the patent with publication No. CN101082120A discloses a method for coating a film on a surface by conical funnel type spiral turning, and the patent with publication No. CN103160795A discloses a method for coating a film on a drum type surface, wherein the three methods all adopt a plasma method to prepare surface modified powder, and the preparation amount of the powder is small under the premise of ensuring uniformity, compactness and purity, and can only meet the micro use requirement, and the preparation requirement of the composite material on modified powder can not be met when the existing equipment on the market is used for about 5 g-30 g each time.
Therefore, a device and a method capable of finishing surface modification of a large amount of micro-nano powder are needed.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a device and a method for modifying the surface of micro-nano powder in order to overcome the defects in the prior art. The device combines vacuum feeding device and storage device through a special vibration stirring mode, has perfectly solved under the prerequisite of guaranteeing homogeneity, compactness, purity requirement, and powder single treatment powder volume is few, and the device is on the basis of current equipment, through selecting different evaporation sources, can realize the preparation of modified materials such as metal, pottery and nonmetal.
In order to solve the technical problems, the invention adopts the following technical scheme: the utility model provides a device at little nanometer powder surface modification, its characterized in that, includes the vacuum chamber, install vibration stirring mechanism in the vacuum chamber, vibration stirring mechanism includes the vibration bowl, the dust guard that opens or close to the vibration bowl is installed on vibration bowl upper portion, vibration bowl mid-mounting has the guide post, the vibrator is installed to vibration bowl downside, the pillar that supports the vibration bowl is still installed to vibration bowl downside, install the evaporation source that handles the inside powder of vibration stirring mechanism on the vacuum chamber, the guide mouth that opens or close through the guide post has been seted up to vibration bowl lower part.
The device for modifying the surface of the micro-nano powder is characterized in that the evaporation source is a magnetic control target source of a magnetic control sputtering device, an electric arc device or an electric arc source of a multi-arc ion plating device, an electron gun or a hollow cathode of a gas plasma device.
The device for modifying the surface of the micro-nano powder is characterized in that the bottom of the vibration bowl is spherical, the material guide column and the material guide opening are both positioned in the center of the bottom of the vibration bowl, the material guide column is in a circular truncated cone shape, and the material guide column is connected with the bottom of the vibration bowl through a clamping groove; a plurality of vibrating blocks for falling off the powder stuck on the inner side wall are arranged on the outer side of the side wall of the vibrating bowl; the vibration bowl is connected with a bias power supply for negatively charging powder in the vibration bowl.
The device for modifying the surface of the micro-nano powder is characterized in that the vacuum cabin is connected with a vacuum assembly for vacuumizing the vacuum cabin and filling protective gas, and an observation window for observing the vibration bowl is formed in the vacuum cabin.
The device for modifying the surface of the micro-nano powder is characterized in that a vacuum feeding assembly is arranged outside the vacuum cabin and comprises a vacuum chamber, a powder chamber and a mechanical telescopic tube extending into or out of a vibration bowl, and the mechanical telescopic tube lifts or drops a guide column.
The device for modifying the surface of the micro-nano powder is characterized in that a storage component is arranged outside the vacuum cabin and comprises a storage chamber and a material guide pipe connecting the storage chamber with a material guide opening.
In addition, the invention provides a method for modifying the surface of micro-nano powder, which is characterized by comprising the following steps:
firstly, filling powder into a vibration bowl, closing a dust baffle plate, and filling the same powder into a vacuum chamber and a powder chamber to obtain a powder-filled modification device;
step two, vacuumizing the vacuum cabin of the modification device filled with the powder obtained in the step one, filling argon, heating the powder in the vibration bowl, and opening a dust baffle plate to obtain the modification device filled with the heated powder;
step three, opening a vibrator and a vibrating block of the modifying device with the heated powder obtained in the step two, so that the powder turns over in a vibrating bowl, and simultaneously, loading a bias power supply to the vibrating bowl to obtain the modifying device with the powder to be modified;
opening an evaporation source of the modification device with the powder to be modified, which is obtained in the step three, modifying the powder, closing the evaporation source after the powder in the vibration bowl is modified, closing the dust plate, moving the material guide column, and enabling the modified powder to enter the material storage chamber through the material guide pipe to obtain modified powder and the modification device;
and fifthly, conveying the powder in the vacuum chamber in the modification device obtained in the step four into a vibration bowl, conveying the powder in the powder chamber into the vacuum chamber, repeating the step two to the step four to modify the powder in the vibration bowl, conveying the powder in the vacuum chamber into the vibration bowl, repeating the step two to the step four to modify the powder in the vibration bowl, and finally obtaining modified powder in a storage chamber.
According to the invention, powder is respectively filled into the vibration bowl, the vacuum chamber and the powder chamber, the powder in the vibration bowl is subjected to modification treatment, the powder in the vacuum chamber is sent into the vibration bowl for modification treatment and then is output after the powder in the vibration bowl is modified and is output, and finally the powder in the powder chamber is sent into the vibration bowl for modification treatment and is output, so that the powder can be continuously added into the powder chamber in the modification process, and the powder modification and output can be continuously carried out under the condition of not damaging the vacuum condition in the vacuum chamber, and the cyclic modification is carried out; the method realizes the surface modification of various powder surfaces of pure metals, alloys, ceramics and the like, and provides infinite possibility for the research of the later-stage material performance.
The method is characterized in that the mass of the powder in the first step is 1 g-2000 g. The invention is not only suitable for modifying a small amount of powder, but also suitable for modifying a large amount of powder, and has higher coating rate which can reach more than 90%.
The method is characterized in that the pressure in the vacuum chamber in the second step is 1.0X10 -4 Pa~5.0×10 -3 Pa, wherein the heating is to heat the powder to 50-400 ℃. The invention ensures the modifying effect by controlling the pressure in the empty cabin, and the purpose of the invention is to increase the binding force between the powder base material and the plated powder, aiming atDifferent powder base materials are different in heating temperature, the powder is easy to ignite when the temperature is too high, and the bonding force is not good when the bonding force is too low.
The method is characterized in that the vibration power of the vibrator and the vibration block in the third step is 5-200W, and the voltage output by the bias power supply is 200-500V. According to the invention, the powder in the vibration bowl is fully mixed and modified by controlling the vibration power of the vibrator and the vibration block, so that the uniformity of modification is ensured, and the powder is prevented from being stuck on the bowl wall of the vibration bowl; the invention controls the voltage output by the bias power supply to lead the micro-nano powder in the vibration bowl to be negatively charged and to attract and accelerate the plasma generated by the evaporation source, thereby accelerating the deposition speed on the powder surface and enhancing the binding force between the modified film and the powder surface.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, a vacuum chamber is used for providing a vacuum environment for the surface modification of micro-nano powder, the micro-nano powder is prevented from being oxidized, the powder is continuously vibrated in a vibration bowl by a vibration stirring mechanism, the powder is vibrated and turned over from inside to outside by the action of a vibrator, the surface of the powder is fully exposed and fully modified by the vibration and turning over of the bottom of the vibration bowl, the high coating rate of the surface modification of the powder is ensured, plasma is excited by an evaporation source, the powder is modified, and the thickness of the powder is accurately controlled by controlling the sputtering time of the plasma and the current of the evaporation source according to the difference of the obtained modified film thickness; a material guide opening which is opened or closed by a material guide column is formed in the lower portion of the vibration bowl and is used for discharging modified powder, so that the powder is convenient to collect.
2. According to the invention, the surface of the micro-nano powder is coated with the metal, alloy or ceramic film by combining a plasma method with a vibration stirring mechanism, so that the purpose of modifying the surface of the powder is achieved, a foundation is laid for preparing a high-performance composite material, and the outer surfaces of the micro-nano powder such as pure metal/alloy/ceramic of a matrix and the large-particle powder are coated with pure metal/alloy/ceramic modified film layers, so that the surface modification of different micro-nano powder is realized, different kinds of modified films can be prepared, and the modified films are divided into metal, ceramic (ceramic phase such as nitride, oxide and carbide) and nonmetal (graphene, carbon film, silicon film and boron nitride BN) according to the different kinds of modified material films, and the preparation process of the modified films with different modified film thicknesses and multiple layers is realized.
3. According to the invention, the vibrator and the vibrating block are arranged to enable the surface of each powder to be fully exposed to plasma, so that uniformity of preparing the modified film is ensured, and the requirement of industrial production is met by combining the vacuum feeding component and the storage component, and the single powder treatment capacity can reach the kilogram level.
4. The method for modifying the surface of the micro-nano powder realizes the surface modification of various powders such as pure metal, alloy, ceramic and the like, and provides infinite possibility for the research of the later-stage material performance.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for modifying the surface of micro-nano powder according to the present invention.
Fig. 2 is a schematic view of the structure of the vacuum chamber of the present invention.
Fig. 3 is a schematic structural view of the vibrating upender of the present invention.
FIG. 4 is an SEM image of a modified powder prepared according to example 1 of the invention.
Reference numerals illustrate:
| 1-a vacuum chamber; | 2-vibrating bowl; | 3-a dust plate; |
| 4-a material guiding column; | 5-a vibrator; | 6, a pillar; |
| 7-evaporating source; | 8, a vibrating block; | 9-bias power supply; |
| 10-a vacuum assembly; | 11-an observation window; | 12-a vacuum chamber; |
| 13-a powder chamber; | 14-mechanical telescopic tube; | 15-a storage chamber; |
| 16-a material guiding pipe. |
Detailed Description
The device for modifying the surface of micro-nano powder is described in detail by an embodiment 1.
Example 1
As shown in fig. 1, 2 and 3, the device for modifying the surface of micro-nano powder in this embodiment includes a vacuum chamber 1, a vibration stirring mechanism is installed in the vacuum chamber 1, the vibration stirring mechanism includes a vibration bowl 2, a dust baffle 3 for opening or closing the vibration bowl 2 is installed on the upper portion of the vibration bowl 2, a material guiding column 4 is installed in the middle of the vibration bowl 2, a vibrator 5 is installed on the lower side of the vibration bowl 2, a supporting column 6 for supporting the vibration bowl 2 is also installed on the lower side of the vibration bowl 2, an evaporation source 7 for processing powder inside the vibration stirring mechanism is installed on the vacuum chamber 1, and a material guiding opening for opening or closing the vibration bowl 2 through the material guiding column 4 is opened on the lower portion of the vibration bowl 2.
The vacuum chamber 1 is used for providing a vacuum environment for the surface modification of the micro-nano powder, the micro-nano powder is prevented from being oxidized, the powder is continuously vibrated in the vibration bowl 2 by the vibration stirring mechanism, the powder is vibrated and turned over from inside to outside by the action of the vibrator 5, the surface of the powder is fully exposed and fully modified by the vibration and turning over of the bottom of the vibration bowl 2, the high coating rate of the surface modification of the powder is ensured, the evaporation source 7 is used for exciting plasmas, the powder is modified, and the thickness of the powder is accurately controlled by controlling the sputtering time of the plasmas and the current of the evaporation source 7 according to the difference of the obtained modified film thickness; a material guide opening which is opened or closed by a material guide column 4 is formed in the lower portion of the vibration bowl 2 and is used for discharging modified powder, so that the powder is convenient to collect.
The strut 6 is a spring strut 6, and the vibration bowl 2 is supported by the spring strut 6, and is damped by a spring.
In this embodiment, the evaporation source 7 is a magnetron target source of a magnetron sputtering apparatus, an arc device or an arc source of a multi-arc ion plating apparatus, an electron gun or a hollow cathode of a gas plasma apparatus. The modification is applied to different powders by using different evaporation sources 7.
In the embodiment, as shown in fig. 1 and 3, the bottom of the vibration bowl 2 is spherical, the material guiding column 4 and the material guiding opening are both positioned at the center of the bottom of the vibration bowl 2, the material guiding column 4 is in a shape of a circular table, and the material guiding column 4 is connected with the bottom of the vibration bowl 2 through a clamping groove; a plurality of vibrating blocks 8 for falling off the powder stuck on the inner side wall are arranged on the outer side of the side wall of the vibrating bowl 2; the vibration bowl 2 is connected with a bias power supply 9 for negatively charging the powder in the vibration bowl 2. The bottom of the vibration bowl 2 is spherical, the material guide column 4 and the material guide opening are positioned at the center of the bottom of the vibration bowl 2, powder in the vibration bowl 2 is concentrated towards the center of the bottom of the vibration bowl 2 under the vibration action and rolls through the material guide column 4, the powder moves in the direction of an arrow in fig. 3, the spherical bottom is convenient for collecting the powder after the modification is finished, the material guide column 4 and the bottom of the vibration bowl 2 are connected through a clamping groove, the connection is tight, the powder cannot leak in the modification process, the material guide column 4 is lifted or put down through a mechanical telescopic pipe 14 of a vacuum feeding assembly, the release of modified powder in the vibration bowl 2 is controlled, the kilogram-level micro-nano powder surface in the vibration bowl 2 is continuously exposed under a plasma substance by adjusting the vibration frequency of a vibration motor, the micro-nano powder surface has nearly the same exposure time, the micro-nano powder surface is coated with a uniform modified film with the same thickness, the vibration block 8 on the side wall of the vibration bowl 2 has no clear requirement, the quantity of the vibration block 8 is increased according to the viscosity degree of the powder on the side wall, the size can be changed according to the actual requirement, and the viscosity degree of the powder can be adhered to the surface of the side wall is high, and the modified powder can be wrapped and the vibration rate is guaranteed; the micro-nano powder in the vibration bowl 2 is negatively charged through the bias power supply 9, and the plasmas such as metal cations or nonmetal cations generated by the evaporation source 7 are attracted and accelerated, so that the deposition speed on the surface of the powder is accelerated, the binding force between the modified film and the surface of the powder is enhanced, and the modification efficiency is improved.
As shown in fig. 1, in the present embodiment, a vacuum module 10 for evacuating the vacuum chamber 1 and filling a protective gas is connected to the vacuum chamber 1, and an observation window 11 for observing the vibration bowl 2 is provided on the vacuum chamber 1. The vibration power of the vibration motor is adjusted by observing the vibration state of the powder through the observation window 11,
as shown in fig. 1 and 3, in the present embodiment, 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 vibration bowl 2, and the mechanical telescopic tube 14 lifts or drops the material guiding column 4. The powder in the vacuum chamber 12 is placed in the vibration bowl 2, the powder to be surface-modified is respectively placed in the vacuum chamber 12 and the powder chamber 13, after the powder surface modification in the vibration bowl 2 is finished, the micro-nano powder in the vacuum chamber 12 is introduced into the vibration bowl 2 through the mechanical telescopic tube 14, then the powder in the powder chamber 13 is introduced into the vacuum chamber 12, vacuumizing is carried out for continuous production, and preparation is made for continuous production.
It should be noted that, there is a gap of 2cm ~3cm between vibration bowl 2 and dust board 3, and when dust board 3 is closed, jack-up the guide pillar from the draw-in groove through guide pipe 16, powder thereby gets into guide pipe 16, and the pipe in this equipment, groove are scalable design, increase the controllability of device.
As shown in fig. 1, in this embodiment, a storage assembly is installed outside the vacuum chamber 1, and the storage assembly includes a storage chamber 15 and a material guiding pipe 16 connecting the storage chamber 15 with a material guiding port. The modified powder is guided into the storage component through the material guide pipe 16, and is vacuum packed through the storage component, so that pollution is avoided. After the powder in the vibration bowl 2 is modified, the material guide column 4 in the vibration bowl 2 is removed, the modified powder enters the material storage chamber 15 through the material guide pipe 16, a vacuum sealing machine is arranged in the material storage chamber 15, the modified powder enters the vacuum packaging bag, and the vacuum packaging bag is vacuumized and packaged, so that the oxidation pollution of the powder is better avoided.
The method for modifying the surface of the micro-nano powder is described in detail by the embodiment 2 to the embodiment 4.
Example 2
The embodiment comprises the following steps:
step one, dividing powder into three equal parts, respectively loading the three equal parts into a vibration bowl 2, a vacuum chamber 12 and a powder chamber 13, and closing a dust baffle 3 to obtain a modification device filled with powder; the powder is Ti powder with the total amount of 150g and the particle diameter of 50 nm-100 nm;
step two, vacuumizing the vacuum chamber 1 of the modification device filled with the powder obtained in the step one, filling argon, heating the powder in the vibration bowl 2, and opening the dust baffle 3 to obtain the modification device filled with the heated powder; the pressure in the vacuum chamber 1 is 1.0X10 -4 Pa, wherein the heating is to heat the powder to 120 ℃;
step three, opening the vibrator 5 and the vibrating block 8 of the modifying device with the heated powder obtained in the step two, so that the powder turns in the vibrating bowl 2, and simultaneously loading the vibrating bowl 2 with a bias power supply 9 to obtain the modifying device with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 5-100W, and the voltage output by the bias power supply 9 is 200V;
step four, opening the evaporation source 7 of the modification device with the powder to be modified, which is obtained in the step three, modifying the powder, closing the evaporation source 7 after the powder in the vibration bowl 2 is modified, closing the dust baffle plate 3, moving the material guide column 4, and enabling the modified powder to enter the material storage chamber 15 through the material guide pipe 16 to obtain modified powder and the modification device; the evaporation source 7 is provided with a direct current power supply for three magnetron sputtering power supplies, adopts a high-purity Cu metal target material, excites Cu ions, adjusts the angles of the three magnetron targets and ensures that the sputtering area of the Cu ions in the vibration bowl 2 is maximum;
fifthly, conveying the powder in the vacuum chamber 12 in the modification device obtained in the step four into the vibration bowl 2, conveying the powder in the powder chamber 13 into the vacuum chamber 12, repeating the step two to the step four to modify the powder in the vibration bowl 2, conveying the powder in the vacuum chamber 12 into the vibration bowl 2, repeating the step two to the step four to modify the powder in the vibration bowl 2, and finally obtaining modified powder in the storage chamber 15.
Through detection, the modified powder prepared by the embodiment is prepared by preparing a metal Cu layer on the surface of Ti powder, the coating rate is more than 92%, and the modified powder can be used for preparing a Ti alloy composite reinforced material, so that the strength and the plasticity are obviously improved.
Fig. 4 is an SEM image of the modified powder prepared in this example, and it can be seen from fig. 4 that the Ti powder surface is coated with an obvious Cu layer, and the coating is uniform and continuous, so that the purpose of modifying the Ti powder surface can be achieved.
Example 3
The embodiment comprises the following steps:
firstly, loading powder into a vibration bowl 2, and closing a dust baffle 3 to obtain a modification device filled with the powder; the powder is 500g, and the grain diameter of the Al is 200-300 mu m 2 O 3 Powder;
step two, vacuumizing the vacuum chamber 1 of the modification device filled with the powder obtained in the step one, filling argon, heating the powder in the vibration bowl 2, and opening the dust baffle 3 to obtain the modification device filled with the heated powder; the pressure in the vacuum chamber 1 is 2.0X10 -3 Pa, wherein the heating is to heat the powder to 100 ℃;
step three, opening the vibrator 5 and the vibrating block 8 of the modifying device with the heated powder obtained in the step two, so that the powder turns in the vibrating bowl 2, and simultaneously loading the vibrating bowl 2 with a bias power supply 9 to obtain the modifying device with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 50-100W, and the voltage output by the bias power supply 9 is 200V;
step four, opening the evaporation source 7 of the modification device with the powder to be modified, which is obtained in the step three, modifying the powder, closing the evaporation source 7 after the powder in the vibration bowl 2 is modified, closing the dust baffle plate 3, moving the material guide column 4, and enabling the modified powder to enter the material storage chamber 15 through the material guide pipe 16, so as to obtain the modified powder in the material storage chamber 15; the evaporation source 7 is three magnetron sputtering power supplies for respectively exciting Cu, zr and Cr.
The modified powder prepared in the embodiment is prepared in the following way through detection 2 O 3 The powder surface is prepared with metal Cu, zr and Cr layers, the coating rate is more than 93%, and the modified powder is a good alloy reinforcing phase, and has obvious reinforcing effect in high-entropy alloy.
Example 4
The embodiment comprises the following steps:
step one, dividing powder into three equal parts, respectively loading the three equal parts into a vibration bowl 2, a vacuum chamber 12 and a powder chamber 13, and closing a dust baffle 3 to obtain a modification device filled with powder; the total amount of the powder is 500g, and the particle size of Ni is 0.5 mm-1 mm 3 Al powder;
step two, vacuumizing the vacuum chamber 1 of the modification device filled with the powder obtained in the step one, filling argon, heating the powder in the vibration bowl 2, and opening the dust baffle 3 to obtain the modification device filled with the heated powder; the pressure in the vacuum chamber 1 is 2.0X10 -3 Pa, the addition ofThe heat is to heat the powder to 200 ℃;
step three, opening the vibrator 5 and the vibrating block 8 of the modifying device with the heated powder obtained in the step two, so that the powder turns over in the vibrating bowl 2 to obtain the modifying device with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 100-200W;
step four, opening the evaporation source 7 of the modification device with the powder to be modified, which is obtained in the step three, modifying the powder, closing the evaporation source 7 after the powder in the vibration bowl 2 is modified, closing the dust baffle plate 3, moving the material guide column 4, and enabling the modified powder to enter the material storage chamber 15 through the material guide pipe 16 to obtain modified powder and the modification device; the evaporation source 7 is a gas plasma generating source and is provided with a corresponding power supply, argon is introduced into the gas plasma generating source to be used as hot electron excitation gas, acetylene gas is introduced into a hot electron outlet to crack the acetylene gas into carbon ions and hydrogen ions, and the carbon ions are deposited on Ni 3 The surface of Al powder forms graphene Gr with SP3 bond, and the graphene Gr is not pure graphene obtained by the existence of hydrogen ions;
fifthly, conveying the powder in the vacuum chamber 12 in the modification device obtained in the step four into the vibration bowl 2, conveying the powder in the powder chamber 13 into the vacuum chamber 12, repeating the step two to the step four to modify the powder in the vibration bowl 2, conveying the powder in the vacuum chamber 12 into the vibration bowl 2, repeating the step two to the step four to modify the powder in the vibration bowl 2, and finally obtaining modified powder in the storage chamber 15.
The modified powder prepared in the embodiment is Ni 3 The coating rate of the graphene layer prepared on the surface of the Al powder is more than 93%, and the graphene has the characteristic of high strength, so that the graphene layer is widely focused on the preparation of high-strength and high-toughness alloy, and the problem of nonuniform distribution of the graphene in powder metallurgy is fundamentally solved by coating the graphene on the surface of the powder in the mode.
Example 5
The embodiment comprises the following steps:
step one, dividing powder into three equal parts, respectively loading the three equal parts into a vibration bowl 2, a vacuum chamber 12 and a powder chamber 13, and closing a dust baffle 3 to obtain a modification device filled with powder; the powder is Ti powder with the total amount of 2000g and the particle diameter of 200 nm-500 nm;
step two, vacuumizing the vacuum chamber 1 of the modification device filled with the powder obtained in the step one, filling argon, heating the powder in the vibration bowl 2, and opening the dust baffle 3 to obtain the modification device filled with the heated powder; the pressure in the vacuum chamber 1 is 5.0X10 -3 Pa, wherein the heating is to heat the powder to 400 ℃;
step three, opening the vibrator 5 and the vibrating block 8 of the modifying device with the heated powder obtained in the step two, so that the powder turns in the vibrating bowl 2, and simultaneously loading the vibrating bowl 2 with a bias power supply 9 to obtain the modifying device with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 150-200W, and the voltage output by the bias power supply 9 is 50V;
step four, opening the evaporation source 7 of the modification device with the powder to be modified, which is obtained in the step three, modifying the powder, closing the evaporation source 7 after the powder in the vibration bowl 2 is modified, closing the dust baffle plate 3, moving the material guide column 4, and enabling the modified powder to enter the material storage chamber 15 through the material guide pipe 16 to obtain modified powder and the modification device; the evaporation source 7 is provided with a direct current power supply for three magnetron sputtering power supplies, adopts a high-purity Cu metal target material, excites Cu ions, adjusts the angles of the three magnetron targets and ensures that the sputtering area of the Cu ions in the vibration bowl 2 is maximum;
fifthly, conveying the powder in the vacuum chamber 12 in the modification device obtained in the step four into the vibration bowl 2, conveying the powder in the powder chamber 13 into the vacuum chamber 12, repeating the step two to the step four to modify the powder in the vibration bowl 2, conveying the powder in the vacuum chamber 12 into the vibration bowl 2, repeating the step two to the step four to modify the powder in the vibration bowl 2, and finally obtaining modified powder in the storage chamber 15.
Through detection, the modified powder prepared by the embodiment is prepared by preparing a metal Cu layer on the surface of Ti powder, the coating rate is more than 92%, and the modified powder can be used for preparing a Ti alloy composite reinforced material, so that the strength and the plasticity are obviously improved.
Example 6
The embodiment comprises the following steps:
step one, dividing powder into three equal parts, respectively loading the three equal parts into a vibration bowl 2, a vacuum chamber 12 and a powder chamber 13, and closing a dust baffle 3 to obtain a modification device filled with powder; the total amount of the powder is 1500g, and the grain diameter is 500-800 mu m of Ti powder;
step two, vacuumizing the vacuum chamber 1 of the modification device filled with the powder obtained in the step one, filling argon, heating the powder in the vibration bowl 2, and opening the dust baffle 3 to obtain the modification device filled with the heated powder; the pressure in the vacuum chamber 1 is 1.0X10 -4 Pa, wherein the heating is to heat the powder to 50 ℃;
step three, opening the vibrator 5 and the vibrating block 8 of the modifying device with the heated powder obtained in the step two, so that the powder turns in the vibrating bowl 2, and simultaneously loading the vibrating bowl 2 with a bias power supply 9 to obtain the modifying device with the powder to be modified; the vibration power of the vibrator 5 and the vibration block 8 is 180-200W, and the voltage output by the bias power supply 9 is 100V;
step four, opening the evaporation source 7 of the modification device with the powder to be modified, which is obtained in the step three, modifying the powder, closing the evaporation source 7 after the powder in the vibration bowl 2 is modified, closing the dust baffle plate 3, moving the material guide column 4, and enabling the modified powder to enter the material storage chamber 15 through the material guide pipe 16 to obtain modified powder and the modification device; the evaporation source 7 is provided with a direct current power supply for three magnetron sputtering power supplies, adopts a high-purity Cu metal target material, excites Cu ions, adjusts the angles of the three magnetron targets and ensures that the sputtering area of the Cu ions in the vibration bowl 2 is maximum;
fifthly, conveying the powder in the vacuum chamber 12 in the modification device obtained in the step four into the vibration bowl 2, conveying the powder in the powder chamber 13 into the vacuum chamber 12, repeating the step two to the step four to modify the powder in the vibration bowl 2, conveying the powder in the vacuum chamber 12 into the vibration bowl 2, repeating the step two to the step four to modify the powder in the vibration bowl 2, and finally obtaining modified powder in the storage chamber 15.
Through detection, the modified powder prepared by the embodiment is prepared by preparing a metal Cu layer on the surface of Ti powder, the coating rate is more than 91%, and the modified powder can be used for preparing a Ti alloy composite reinforced material, so that the strength and the plasticity are obviously improved.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (9)
1. The device for modifying the surface of the micro-nano powder is characterized by comprising a vacuum cabin (1), wherein a vibration stirring mechanism is arranged in the vacuum cabin (1), the vibration stirring mechanism comprises a vibration bowl (2), a dust baffle (3) for opening or closing the vibration bowl (2) is arranged at the upper part of the vibration bowl (2), a material guide column (4) is arranged in the middle of the vibration bowl (2), a vibrator (5) is arranged at the lower side of the vibration bowl (2), a support column (6) for supporting the vibration bowl (2) is also arranged at the lower side of the vibration bowl (2), an evaporation source (7) for processing powder in the vibration stirring mechanism is arranged on the vacuum cabin (1), a material guide opening for opening or closing the vibration bowl (2) through the material guide column (4) is arranged at the lower part of the vibration bowl (2), the material guide column (4) and the material guide opening are both positioned at the center of the bottom of the vibration bowl (2), the material guide column (4) is in a shape and is connected with the bottom of the vibration bowl (2) through a clamping groove (4); a plurality of vibrating blocks (8) for falling off the powder stuck on the inner part of the side wall are arranged on the outer part of the side wall of the vibrating bowl (2); the vibration bowl (2) is connected with a bias power supply (9) for negatively charging powder in the vibration bowl (2).
2. The device for modifying the surface of micro-nano powder according to claim 1, wherein the evaporation source (7) is a magnetron target source of a magnetron sputtering device, an electric arc device or an electric arc source of a multi-arc ion plating device, an electron gun or a hollow cathode of a gas plasma device.
3. The device for modifying the surface of the micro-nano powder according to claim 1, wherein the vacuum chamber (1) is connected with a vacuum assembly (10) for vacuumizing and filling protective gas into the vacuum chamber (1), and an observation window (11) for observing the vibration bowl (2) is formed in the vacuum chamber (1).
4. The device for modifying the surface of the micro-nano powder according to claim 1, wherein a vacuum feeding assembly is arranged outside the vacuum chamber (1), the vacuum feeding assembly comprises a vacuum chamber (12), a powder chamber (13) and a mechanical telescopic tube (14) extending into or out of the vibration bowl (2), and the mechanical telescopic tube (14) lifts or drops the material guiding column (4).
5. The device for modifying the surface of the micro-nano powder according to claim 1, wherein a storage component is arranged outside the vacuum chamber (1), and the storage component comprises a storage chamber (15) and a material guiding pipe (16) for connecting the storage chamber (15) with a material guiding opening.
6. A method for modifying the surface of micro-nano powder by using the device as claimed in any one of claims 1 to 5, which comprises the following steps:
firstly, powder is filled into a vibration bowl (2), a dust baffle (3) is closed, and the same powder is filled into a vacuum chamber (12) and a powder chamber (13), so that a powder-filled modifying device is obtained;
step two, vacuumizing the vacuum chamber (1) of the modification device filled with the powder obtained in the step one, filling argon, heating the powder in the vibration bowl (2), and opening the dust baffle (3) to obtain the modification device filled with the heated powder;
step three, opening a vibrator (5) and a vibrating block (8) of the modifying device with the heated powder obtained in the step two, so that the powder turns in a vibrating bowl (2), and simultaneously loading a bias power supply (9) on the vibrating bowl (2) to obtain the modifying device with the powder to be modified;
step four, opening an evaporation source (7) of the modification device with the powder to be modified, which is obtained in the step three, modifying the powder, closing the evaporation source (7) after the powder in the vibration bowl (2) is modified, closing the dust plate (3), moving the material guide column (4), and enabling the modified powder to enter the material storage chamber (15) through the material guide pipe (16) to obtain modified powder and the modification device;
step five, delivering the powder in the vacuum chamber (12) in the modification device obtained in the step four into the vibration bowl (2), delivering the powder in the powder chamber (13) into the vacuum chamber (12), repeating the steps two to four to modify the powder in the vibration bowl (2), delivering the powder in the vacuum chamber (12) into the vibration bowl (2), repeating the steps two to four to modify the powder in the vibration bowl (2), and finally obtaining modified powder in the storage chamber (15).
7. The method according to claim 6, wherein the mass of the powder in the first step is 1g to 2000g.
8. The method according to claim 6, wherein the pressure in the vacuum chamber (1) in step two is 1.0 x 10 -4 Pa～5.0×10 -3 Pa, wherein the heating is to heat the powder to 50-400 ℃.
9. The method according to claim 6, wherein the vibration power of the vibrator (5) and the vibration block (8) in the third step is 5W to 200W, and the voltage outputted from the bias power supply (9) is 200V to 500V.
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