CN112538606A - Surface treatment device and surface modification method for powder material - Google Patents
Surface treatment device and surface modification method for powder material Download PDFInfo
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- CN112538606A CN112538606A CN202011244227.2A CN202011244227A CN112538606A CN 112538606 A CN112538606 A CN 112538606A CN 202011244227 A CN202011244227 A CN 202011244227A CN 112538606 A CN112538606 A CN 112538606A
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- 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
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Abstract
The invention discloses a surface treatment device for powder materials, which comprises a vacuum cavity and a reticular metal fence arranged in the vacuum cavity, wherein a rotating device and an arc-shaped sample table arranged on the rotating device are arranged in the reticular metal fence; the top of the net-shaped metal fence is provided with a net cover which covers the net-shaped metal fence; the vacuum chamber further comprises a heating device arranged on the inner side wall of the vacuum chamber body, a fan arranged right above the mesh enclosure and a power supply used for providing an electric field. The invention also discloses a method for carrying out plasma surface modification on the powder material by adopting the surface treatment device. The processing device can realize the effective deposition and coating of the metal/nonmetal/metal compound/nonmetal compound sputtering target material on the surface of the powder material.
Description
Technical Field
The invention relates to a surface treatment device for powder materials, and also relates to a method for performing plasma surface modification on the powder materials by adopting the surface treatment device.
Background
With the rapid development of society, the requirements of various industries on material performance are continuously improved, the traditional materials are difficult to meet the requirements, and for example, the development of a single powder material in the fields of powder metallurgy, energy industry, 3D printing and other industries is limited to a certain extent. In order to solve the problem, researchers have realized the improvement of the physicochemical properties of the powder material by modification methods such as a sol-gel method, a high-temperature solid phase method, a chemical plating method, a vapor deposition method and the like, wherein the plasma surface modification method receives more attention due to its low price, environmental protection and high efficiency, the plasma surface modification method realizes the surface modification of the powder material by means of defects, nanocrystallization, compounding and the like, but the current plasma surface modification method has the problems of poor stability of the surface defects of the powder material (poor stability means that no deposition coating is formed on part of the powder), low yield, uneven sputtering and the like, so that the commercialization process is difficult to promote.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides a surface treatment device for a powder material and a method for performing plasma surface modification on the powder material by adopting the surface treatment device, aiming at the problems of poor stability of powder material surface defects, low yield, uneven sputtering and the like in a plasma surface modification method in the prior art.
The technical scheme is as follows: the surface treatment device for the powder material comprises a vacuum cavity and a reticular metal fence arranged in the vacuum cavity, wherein a rotating device and an arc-shaped sample table arranged on the rotating device are arranged in the reticular metal fence, and the powder material is arranged in the arc-shaped sample table; the top of the net-shaped metal fence is provided with a net cover which covers the net-shaped metal fence; the vacuum chamber further comprises a heating device arranged on the inner side wall of the vacuum chamber body, a fan arranged right above the mesh enclosure and a power supply used for providing an electric field.
Wherein, the vacuum cavity further comprises an air inlet and an air outlet.
The mesh enclosure is in the shape of an inwards concave arc, an outwards convex arc or a flat plate, and is made of one sputtering material or a plurality of sputtering materials in a matching way.
The vertical distance between the center point of the mesh enclosure and the upper end face of the powder material in the arc-shaped sample table is 1-5 cm, the mesh enclosure is in a mesh shape or is formed by splicing a plurality of sheet-shaped sputtering materials, and a gap is reserved between each sheet of sheet-shaped sputtering material.
The method for performing plasma surface modification on the powder material by adopting the surface treatment device for the powder material comprises the following steps: placing an arc-shaped sample table with powder materials on a rotating device, wherein the thickness of the powder materials in the arc-shaped sample table is 0.1-0.5 mm, covering a mesh enclosure, closing a vacuum cavity, vacuumizing to below 1-2 MPa, closing a molecular pump, introducing ionizable gas, igniting to generate glow, adjusting the voltage to 550-700V, the duty ratio to 37-55%, raising the temperature to 350-600 ℃, performing plasma deposition, and starting the rotating device to rotate the powder materials after the temperature reaches 350-600 ℃; and (4) closing the power supply after the constant-temperature deposition time is 4-6 hours, and naturally cooling to room temperature to obtain the powder composite material.
The powder composite material is a powder composite material with nano particles embedded on the surface or a powder composite material with a metal, nonmetal or metal and nonmetal compound nano coating coated on the surface.
Wherein, the mesh enclosure is a sputtering target material of metal, nonmetal, metal compound or nonmetal compound.
Wherein the ionizable gas is one or more of hydrogen, argon, nitrogen-containing gas or carbon-containing gas.
Wherein the powder material is in a discrete structure, and the particle size of the powder material is 5 nm-1 mm.
The mechanism analysis of the invention is as follows: the device disclosed by the invention sputters the metal of the net cover in the process of moving the plasma to the material, sputtered particles react with particles in the plasma or are deposited on the surface of the sample along with the reaction, and the rotating device overturns the sample to ensure the treatment uniformity and realize coating, namely the coating of the nano coating on the surface of the powder material.
Has the advantages that: the processing device can realize the effective deposition and coating of the metal/nonmetal/metal compound/nonmetal compound sputtering target material on the surface of the powder material, and can simultaneously coat more samples in the sputtering process due to the arrangement of the overturning platform, and the processing time is short.
Drawings
FIG. 1 is a schematic structural diagram of a powder material surface treatment apparatus according to the present invention;
fig. 2 is a schematic structural view of a mesh-shaped metal fence and an arc-shaped mesh enclosure cooperatively connected with the mesh-shaped metal fence;
FIG. 3 is a scanning electron micrograph of the powder composite of example 1 according to the present invention;
FIG. 4 is a scanning electron micrograph of a powder composite material according to example 2 of the present invention;
FIG. 5 is an energy spectrum of the polymer particles and copper composite in example 2 of the present invention.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments.
As shown in fig. 1-2, the surface treatment device for powder materials of the present invention comprises a vacuum chamber 1 and a mesh-shaped metal fence 3 disposed in the vacuum chamber 1, wherein a rotating device and an arc-shaped sample stage 5 fixed on the rotating device 4 are disposed in the mesh-shaped metal fence 3, and a powder material 10 is disposed in the arc-shaped sample stage 5; the rotating device 4 comprises a first driving motor, a rotating shaft I4-1 and a second driving motor which are fixedly connected with an output shaft of the first driving motor, and a rotating shaft II4-2 which is fixedly connected with an output shaft of the second driving motor, wherein the fixed ends of the first driving motor and the second driving motor are fixed in the vacuum cavity 1, and the bottom surface of the arc-shaped sample table 5 is fixed on the rotating shaft I4-1 and the rotating shaft II 4-2; when the first driving motor and the second driving motor rotate forwards simultaneously, the rotating shaft I4-1 and the rotating shaft II4-2 rotate towards the right simultaneously (the rotating angle towards the right is within 30 degrees), the arc-shaped sample stage 5 is driven to turn towards the right, the first driving motor and the second driving motor return to the initial positions simultaneously and then rotate backwards simultaneously, the rotating shaft I4-1 and the rotating shaft II4-2 rotate towards the left simultaneously (the rotating angle towards the left is within 30 degrees), the arc-shaped sample stage 5 is driven to turn towards the left, the motor rotates forwards and rotates backwards for 30 degrees repeatedly, and therefore the arc-shaped sample stage 5 is driven to turn left and right repeatedly; the top of the reticular metal fence 3 is provided with a mesh enclosure 2, the mesh enclosure 2 covers the reticular metal fence 3, and the mesh enclosure 2 is positioned right above the arc-shaped sample table 5; the surface treatment device for the powder material further comprises a heating device 7 arranged on the inner side wall of the vacuum cavity 1, a fan 11 arranged right above the mesh enclosure 2 and a power supply 12 for providing an electric field, wherein the fan 11 can increase the transmission efficiency of ions from the mesh enclosure 2 to the powder material 10; the heating device 7 is an electric heating plate; the vacuum chamber 1 further comprises a gas inlet 8 and a gas outlet 9, wherein the ionizable gas enters the vacuum chamber 1 through the gas inlet 8 and is exhausted through the gas outlet 9. The shape of the mesh enclosure 2 is an inward concave arc shape, an outward convex arc shape or a flat plate shape, and the mesh enclosure 2 is made of one sputtering material or a mixture of a plurality of sputtering materials. The vertical distance A between the center point of the mesh enclosure 2 and the upper end face of the powder material 10 in the arc-shaped sample table 5 is 1-5 cm, the mesh enclosure 2 is in a mesh shape or is formed by splicing a plurality of sheet-shaped sputtering materials, and a gap is reserved between each sheet of sheet-shaped sputtering material. Except for the mesh enclosure 2, the arc-shaped sample table 5, the rotating device shell and the reticular metal fence 3 are all made of materials difficult to sputter. In addition, the net-shaped metal fence 3 with the net cover 2 on the top can enable the powder material to form a heat accumulation effect in the processing process, and temperature uniformity is guaranteed.
Example 1
The method for performing plasma surface modification on the powder material by adopting the surface treatment device for the powder material comprises the following steps: cleaning the arc-shaped sample table 5 and the surrounding environment by using deionized water and alcohol by using radio frequency plasma deposition equipment, and removing residual particle impurities by using a dust collector; spreading a carbon material on an arc-shaped sample table 5 by using a sieve, wherein the thickness of the carbon material in the arc-shaped sample table 5 is 0.1-0.5 mm, covering a mesh enclosure 2, the mesh enclosure 2 is an inward concave arc-shaped mesh enclosure 2, the mesh enclosure 2 is prepared by porous silicon, the vertical distance A between the center point of the mesh enclosure 2 and the upper surface of the carbon material 10 is 5cm, closing a vacuum cavity 1, vacuumizing to the vacuum degree below 1MPa, closing a molecular pump, introducing 99.999% nitrogen gas of 150sccm, striking an arc to generate glow, adjusting the voltage to 550-700V, adjusting the duty ratio to 55%, raising the temperature to 450 ℃, performing plasma deposition, starting a rotating device to rotate a powder material to ensure the deposition uniformity after the temperature reaches 450 ℃, starting a fan, setting a bias voltage 14 to-30V (the bias voltage is used for improving the energy of charged particles in the plasma, sputtering of high-energy particles to the mesh enclosure is more obvious, and can help the ions to rapidly move to the surface of, therefore, the bias voltage can increase the ion sputtering and deposition efficiency), the power supply is turned off after the constant-temperature deposition time is 3 hours, the temperature is reduced, the chamber is naturally cooled to the room temperature, the pressure cavity force is consistent with the air pressure, and the sample loss is reduced.
In example 1, the powder material is an ordered mesoporous carbon material, and the sputterable material is a porous silicon target material. The morphology of the powder composite material prepared in example 1 is characterized, and as shown in fig. 3, the powder composite material prepared in example 1 is: the ordered mesoporous carbon has homogeneously dispersed nanometer grains in the surface and pores.
Example 2
Example 2 the apparatus used in example 1 was the same except that the mesh cap 2 was a flat plate type, and the mesh cap 2 was made of a copper alloy. The polytetrafluoroethylene particles are spread on an arc-shaped sample table 5 by using a sieve, the thickness of the polytetrafluoroethylene particles in the arc-shaped sample table 5 is 0.1 mm, so that the deposition uniformity is ensured, and the vertical distance between the upper surface of the sample and the central point of a mesh enclosure 2 is 1 cm; closing the vacuum cavity 1, vacuumizing to below 1MPa, closing the molecular pump, introducing 99.999 percent nitrogen gas of 100sccm, striking an arc to generate glow, adjusting the voltage to 500V, adjusting the duty ratio to 74 percent, raising the temperature to 550 ℃, and performing plasma deposition; and when the temperature reaches 550 ℃, starting a rotating device to rotate the powder material to ensure the deposition uniformity, starting a fan, setting the bias voltage to be 14-50V, closing a glow power supply after the constant-temperature deposition time is 2 hours, carrying out cooling treatment, naturally cooling to room temperature, keeping the pressure of the pressure chamber consistent with the air pressure, and reducing the sample loss.
The morphology of the powder composite material prepared in example 2 is characterized, and as shown in fig. 4 to 5, the powder composite material prepared in example 2 is: the polytetrafluoroethylene particles are wrapped with Cu coatings.
Claims (9)
1. A surface treatment device for powder materials is characterized in that: the vacuum powder material powder; the top of the net-shaped metal fence is provided with a net cover which covers the net-shaped metal fence; the vacuum chamber further comprises a heating device arranged on the inner side wall of the vacuum chamber body, a fan arranged right above the mesh enclosure and a power supply used for providing an electric field.
2. The surface treatment apparatus for a powder material according to claim 1, wherein: the vacuum chamber further comprises an air inlet and an air outlet.
3. The surface treatment apparatus for a powder material according to claim 1, wherein: the shape of the mesh enclosure is an inward concave arc shape, an outward convex arc shape or a flat plate shape, and the mesh enclosure is made of one sputtering material or a mixture of multiple sputtering materials.
4. The surface treatment apparatus for a powder material according to claim 1, wherein: the vertical distance between the center point of the mesh enclosure and the upper end face of the powder material in the arc-shaped sample table is 1-5 cm, the mesh enclosure is in a mesh shape or is formed by splicing a plurality of sheet sputtering materials, and a gap is reserved between each sheet sputtering material.
5. A method for performing plasma surface modification on a powder material by using the surface treatment device for a powder material according to claim 1, which is characterized by comprising the following steps: placing an arc-shaped sample table with powder materials on a rotating device, wherein the thickness of the powder materials in the arc-shaped sample table is 0.1-0.5 mm, covering a mesh enclosure, closing a vacuum cavity, vacuumizing to below 1-2 MPa, closing a molecular pump, introducing ionizable gas, igniting to generate glow, adjusting the voltage to 550-700V, the duty ratio to 37-55%, raising the temperature to 350-600 ℃, performing plasma deposition, and starting the rotating device to rotate the powder materials after the temperature reaches 350-600 ℃; and (4) closing the power supply after the constant-temperature deposition time is 4-6 hours, and naturally cooling to room temperature to obtain the powder composite material.
6. The method for performing plasma surface modification on a powder material by using the surface treatment device for a powder material according to claim 5, wherein: the powder composite material is a powder composite material with nano particles embedded on the surface or a powder composite material with a metal, nonmetal or metal and nonmetal compound nano coating coated on the surface.
7. The method for performing plasma surface modification on a powder material by using the surface treatment device for a powder material according to claim 5, wherein: the mesh enclosure is a metal, nonmetal, metal compound or nonmetal compound sputtering target material.
8. The method for performing plasma surface modification on a powder material by using the surface treatment device for a powder material according to claim 5, wherein: the ionizable gas is one or more of hydrogen, argon, nitrogen-containing gas or carbon-containing gas.
9. The method for performing plasma surface modification on a powder material by using the surface treatment device for a powder material according to claim 5, wherein: the powder material is in a discrete structure, and the particle size of the powder material is 5 nm-1 mm.
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| CN202011244227.2A CN112538606B (en) | 2020-11-09 | 2020-11-09 | Surface treatment device and surface modification method for powder material |
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| CN202011244227.2A CN112538606B (en) | 2020-11-09 | 2020-11-09 | Surface treatment device and surface modification method for powder material |
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Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TW201121642A (en) * | 2009-12-23 | 2011-07-01 | Metal Ind Res & Dev Ct | Material stirring mechanism applicable to drum type equipment. |
| TW201226619A (en) * | 2010-12-16 | 2012-07-01 | Metal Ind Res & Dev Ct | Compound roller mechanism of sputtering apparatus |
| CN105312554A (en) * | 2014-07-07 | 2016-02-10 | 张家港市超声电气有限公司 | Method for performing powder material surface modification through plasma |
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