CN112538606B - 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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- CN112538606B CN112538606B CN202011244227.2A CN202011244227A CN112538606B CN 112538606 B CN112538606 B CN 112538606B CN 202011244227 A CN202011244227 A CN 202011244227A CN 112538606 B CN112538606 B CN 112538606B
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- 239000000843 powder Substances 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 63
- 238000004381 surface treatment Methods 0.000 title abstract description 14
- 238000002715 modification method Methods 0.000 title description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 230000008021 deposition Effects 0.000 claims abstract description 16
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 12
- 230000004048 modification Effects 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 10
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 230000005684 electric field Effects 0.000 claims abstract description 4
- 238000005477 sputtering target Methods 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002103 nanocoating Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000004544 sputter deposition Methods 0.000 description 13
- 239000003575 carbonaceous material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910021426 porous silicon Inorganic materials 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C23C14/34—Sputtering
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明公开了一种粉体材料的表面处理装置，包括真空腔体以及设置在真空腔体内的网状金属围栏，所述网状金属围栏内设有转动装置以及放置在转动装置上的弧形样品台，粉体材料置于弧形样品台中；所述网状金属围栏顶部设有网罩，网罩罩在网状金属围栏上；还包括设置在真空腔体内侧壁上的加热装置、设置在网罩正上方的风机以及用于提供电场的电源。本发明还公开了采用上述表面处理装置对粉体材料进行等离子体表面改性的方法。本发明处理装置能够实现金属/非金属/金属化合物/非金属化合物溅射靶材在粉体材料表面的有效沉积与包覆。
The invention discloses a surface treatment device for powder materials, comprising a vacuum cavity and a mesh metal fence arranged in the vacuum cavity. The mesh metal fence is provided with a rotating device and an arc-shaped arc placed on the rotating device. The sample table, the powder material is placed in the curved sample table; the top of the mesh metal fence is provided with a mesh cover, and the mesh cover is covered on the mesh metal fence; it also includes a heating device arranged on the inner side wall of the vacuum chamber, a The fan just above the grille and the power supply for the electric field. The invention also discloses a method for performing plasma surface modification on powder materials by using the above-mentioned surface treatment device. The processing device of the invention can realize the effective deposition and coating of the metal/non-metal/metal compound/non-metal compound sputtering target 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 the material, 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 (4)
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2020
- 2020-11-09 CN CN202011244227.2A patent/CN112538606B/en active Active
Patent Citations (9)
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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 |
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