CN103160795A - Target magnetron sputtering device and film coating method used for powder particle surface film coating - Google Patents
Target magnetron sputtering device and film coating method used for powder particle surface film coating Download PDFInfo
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- CN103160795A CN103160795A CN2011104275531A CN201110427553A CN103160795A CN 103160795 A CN103160795 A CN 103160795A CN 2011104275531 A CN2011104275531 A CN 2011104275531A CN 201110427553 A CN201110427553 A CN 201110427553A CN 103160795 A CN103160795 A CN 103160795A
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Abstract
The invention provides a target magnetron sputtering device and a film coating method used for powder particle surface film coating. The target magnetron sputtering device comprises a vacuum chamber, a roller with openings at two ends, two support rollers, a motor, a speed regulation device, two magnetron sputtering target frames and a sputtering power source, wherein each support roller is provided with a limiting inclined face. The support rollers are connected with the speed regulation device. The roller is directly placed on the support rollers and driven to rotate through the support rollers. Target materials are arranged at the positions of the openings at the two ends of the roller. During magnetron sputtering film coating, a grinding ball and powder are simultaneously placed into the roller, the rotating speed of the motor is regulated, the grinding ball and powder particles in the roller are enabled to drop in a parabola mode, sputtering stream injected from the openings of the roller is deposited on the falling powder, and film with good evenness is obtained after a certain period of time. The target magnetron sputtering device and the film coating method used for the powder particle surface film coating are large in technological handling capacity, low in operational cost and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of powder granule surface coating technique, be specifically related to be applicable to vacuum coater and the method for dynamic magnetron sputtering plating.
Background technology
Along with the progress of science and technology and developing rapidly of new material industry, people are to the requirement of powder characteristic also corresponding improving constantly.By methods such as physics, chemistry, machineries, powder body material surface or interface are processed, can be improved or change the performance of powder body material, satisfy the needs of novel material, novel process and development of new techniques.Wherein, the surface coating technology is to use maximum powder surface treatment technologies.
The method of powder granule surface coating mainly contains electroless plating, plating, vacuum sputtering plating, vacuum evaporation, chemical vapour deposition and sol-gel method etc.Adopt the chemical process plated films such as electroless plating, plating, sol-gel method, institute obtains that the powder surface film is inhomogeneous, compactness is poor, purity is low, and the material system of superficial film is restricted, owing to will adopting chemical agent also easily to cause environmental pollution.Adopt the physical methods such as vacuum sputtering coating (hereinafter to be referred as " sputter plating "), vacuum evaporation deposition plated film (hereinafter to be referred as " evaporation ") not need to adopt chemical agent, institute's powder surface film purity that obtains is high and do not have environmental pollution, is subject to increasing application.
During the physical methods such as employing sputter plating and evaporation, in order to obtain the film of good uniformity at powder surface, need to allow each particle have the chance of being equal to fully to expose its surface when film growth, and the deposition probability that makes as far as possible the target as sputter of powder granule surface all directions go out material equate.Patent CN1718845A, patent CN101798677A and patent CN201665704U disclose a kind of powder granule magnetron sputtering coating method that adopts vertical shaft type ultrasonic vibration sample table.The method single treatment amount is little, only can satisfy scientific research and laboratory needs.Patent CN101082120A discloses the Processes and apparatus that a kind of powder surface carries out plated film.It is by making the powder motion of spinning in conical hopper, to reach the even exposure of powder granule in the sputter field.The thickness of this equipment plated film is relatively fixing, difficult adjusted and only have a target can not realize cosputtering.The horizontal axis drum-type sample stage that patent CN101805893A provides magnetron sputtering to use, it comprises vibration of ultrasonic wave mechanism and screen cloth etc., the even and coating film thickness of its plated film is easily adjusted, but its complicated structure, and can only the one direction sputter coating.
Summary of the invention
For the problems referred to above of prior art, the invention provides a kind of facing-target magnetron sputtering system device and film coating method thereof of powder granule surface coating, this technology can plate the uniform film of one deck on the powder granule surface, and two kinds of mould materials of sputter simultaneously.
For achieving the above object, the present invention includes following technical scheme:
A kind of facing-target magnetron sputtering system device for the powder granule surface coating, this device comprise the cylinder of vacuum chamber, both ends open, two supporting rolls with spacing inclined-plane, motor and speed regulation device, two magnetron sputtering target holders and shielding power supply; Wherein, this supporting roll is connected with motor and speed regulation device, the axial level of each supporting roll, is parallel to each other and is positioned at the par height; This drum shaft is to lying in a horizontal plane on supporting roll, load in cylinder powder granule and/or with the mill ball of the identical material of powder; These two magnetron sputtering target holders are placed in respectively the both ends open outside of this cylinder, place target on target holder, and axle center and the cylinder of target are axially aligned; This vacuum chamber is connected with vacuum suction device, and viewing window and purging valve are set on vacuum chamber, and this cylinder, supporting roll and target holder are placed in vacuum chamber.
Device as above, wherein, the opening part edge of this cylinder can be formed slopely the inclined-plane to the inside, and tilt angle theta is 120～160 degree, the inner diameter d of cylinder opening part
1=d
2/ 3～3d
2/ 4, wherein, d
2Be the cylinder internal diameter.
Device as above, wherein, the length of this supporting roll is identical with drum length, and the angle of inclination on its spacing inclined-plane is identical with the tilt angle theta of the opening part bezel of described cylinder.
Device as above, wherein, the outside diameter d of this supporting roll
3=(d
2+ δ)/2～3 (d
2+ δ)/2, δ is the wall thickness of cylinder, the spacing surface width b of supporting roll
1=b
2/ 3～b
2, b
2Surface width for the cylinder opening part.
Device as above wherein, is provided with fin equably on the inwall of this cylinder, the trend of fin and cylinder axially parallel, and the quantity of fin is 4～12, the height h=d of fin
2/ 25d
2/ 5, the width a=h/6～h of fin.
Device as above, wherein, the distance between this sputter target holder and cylinder opening part is 3cm～20cm.
Device as above, wherein, surface-coated one deck nonskidcoating of this supporting roll.
On the other hand, the present invention includes and use device as above to the method for powder granule surface coating, comprise the steps:
A. open vacuum chamber, powder granule and mill ball are put into cylinder, cylinder is placed on support roller;
B. required target is arranged on target holder, and is alignd with the axle center of cylinder in the axle center of target;
C. close vacuum chamber, open vacuum suction device, the vacuum of vacuum chamber is extracted into 1 * 10
-4Pa～8 * 10
-3Pa;
D. be filled with argon gas to vacuum chamber, control flow with mass flowmeter, when guaranteeing sputter, the vacuum chamber operating air pressure is 0.2Pa～2Pa;
E. open motor, support roller rotarily drives rollers roll, and the rotating speed of regulating electric machine makes mill ball and powder granule in cylinder be para-curve;
F. open shielding power supply, regulating power makes power on the target unit surface at 2W/cm
2～6W/cm
2, the beginning sputter coating;
G. after reaching the thickness of the film that needs sputter, close the power supply of target, stop sputter;
F. close in order under meter, vacuum system, open purging valve and slowly exit in vacuum chamber, after vacuum room pressure and barometric point balance, open vacuum chamber, take out cylinder, mill ball and powder are sieved, obtain the powder of plated film.
Method as above, wherein, the material of this mill ball is identical with the material of powder, perhaps can not pollute powder, and the diameter of mill ball is 3～20mm.
Method as above, wherein, the mass ratio of this powder and mill ball is 0.2～3: 1, the cumulative volume of powder and mill ball is no more than 45% of cylinder volume.
Method as above, wherein, the speed adjustment scope of this cylinder is 0.5～0.96 times of quick passage critical speed, quick passage critical speed is
Rev/min kind, d
2Be the internal diameter of cylinder, unit is m.
Method as above, wherein, the distance between this sputter target holder and cylinder opening part is 3cm～20cm.
Method as above, wherein, the particle diameter of this powder granule can be 0.1～2000 μ m.
Beneficial effect of the present invention is: this device adopts the horizontal axis drum-type sample stage of both ends open, be put in cylinder with mill ball and the powder granule of the identical material of powder, the speed of rotation of regulating cylinder is brought to above cylinder mill ball and powder granule, be para-curve under action of gravitation, the plasma sputtering corradiation district that forms by the relative target in two ends will at powder surface deposition targets material, can plate the uniform film of one deck through the certain hour powder surface.Mill ball grinds powder, destroys the reunion of powder, and mill ball can play the effect of vibration, is come out fully in the surface of powder granule, is conducive to the film at powder granule surface deposition good uniformity.Fin by in inner wall of rotary drum welding some amount drives the rotation of mill ball and powder better, improves the efficient of plated film.Apparatus and method of the present invention can be carried out target co-sputtering, and two kinds of mould materials of sputter simultaneously also can two a kind of materials of target sputter simultaneously, when a kind of material of sputter, can improve the efficient of plated film.
In sum, apparatus structure of the present invention is simple, operating procedure is easy, running cost is low, processes that the powder amount is large, efficient is high, make the powder plated film evenly, fine and close, purity is high, is fit to industrial production.
Description of drawings
Fig. 1 is the facing-target magnetron sputtering system apparatus structure schematic diagram that the embodiment of the present invention 1 is used for the powder granule surface coating.
Fig. 2 is that Fig. 1 is along the A-A sectional view.
Fig. 3 is the optical microscope photograph of the copper plating film glass powder of the embodiment of the present invention 2 preparations.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1 is used for the facing-target magnetron sputtering system device of powder granule surface coating
Referring to illustrated in figures 1 and 2, in a kind of preferred implementation of the present invention, this magnetic control sputtering film plating device comprises the cylinder 2 of vacuum chamber 1, both ends open, two supporting rolls 3 with spacing inclined-plane, motor and speed regulation device 4, two magnetron sputtering target holders 5 and shielding power supply 6.
Wherein, supporting roll 3 is connected with motor and speed regulation device 4, the two axial levels of supporting roll 3, is parallel to each other and is positioned at the par height.Supporting roll 3 axial lengths are 20cm, the outside diameter d of supporting roll
3Be 8cm, the tilt angle theta on supporting roll spacing inclined-plane is 145 °, the spacing surface width b of supporting roll
1Be 2cm.
The wall thickness δ of cylinder is 0.2cm, and axial length is 20cm, inner diameter d
2Be 12cm.The opening part edge of cylinder is formed slopely the inclined-plane to the inside, and tilt angle theta is 145 °, the inner diameter d of cylinder opening part
1Be 85mm.Cylinder 2 axially lies in a horizontal plane on supporting roll 3, and the spacing inclined-plane at the two ends of supporting roll plays resting barrel.Drive supporting rolls 3 rotations by motor and speed regulation device 4, the friction by 2, support roller 3 and cylinder etc. interacts and drives cylinder 2 and rotate.In order to increase the friction of 2, supporting roll 3 and cylinder, prevent from skidding, the surface of supporting roll 3 is coated with the last layer nonskidcoating.The interior loading powder granule of cylinder 2 and/or with the mill ball of the identical material of powder.Be provided with equably fin 7 on the inwall of cylinder, the trend of fin 7 and cylinder 2 axially parallels, the quantity of fin is 8, and height h is 8mm, and width a is 3mm.
Two magnetron sputtering target holders 5 are placed in respectively the both ends open outside of this cylinder 2, and the distance between magnetron sputtering target holder 5 and cylinder opening part is 3cm～20cm, and magnetron sputtering target holder 5 is connected with shielding power supply 6.Place target on target holder 5, axle center and the cylinder of target are axially aligned.
Vacuum chamber 1 is connected with vacuum suction device 8, and viewing window 9 and purging valve 10 are set on vacuum chamber 1, the convenient starting the arc of target, the motion conditions of powder granule of observing of viewing window, configuration quality under meter, electrical equipment control and cooling circulating water system simultaneously.Cylinder 2, supporting roll 3 and two target holders 5 are placed in vacuum chamber 1.
Embodiment 2 adopts the described devices of embodiment 1 to carry out the magnetron sputtering tin-copper alloy film WU to solid glass ball powder granule surface
Processing step is as follows:
1. opening vacuum chamber, is that 50 μ m solid glass ball powder granules and 150 gram glass grinding balls are put into cylinder with 150 gram particle degree, and cylinder is placed in to be supported to roll on, and the diameter of glass grinding ball is 4mm; Required two copper targets are arranged on target holder respectively, and are alignd with the axle center of cylinder in the axle center of target;
2. close vacuum chamber, open vacuum suction device, the vacuum of vacuum chamber is extracted into 0.5 * 10
-3Pa;
3. be filled with argon gas to vacuum chamber, control flow with mass flowmeter, when guaranteeing sputter, the vacuum chamber operating air pressure is 0.5Pa;
4. unlatching motor, the rotating speed of regulating electric machine makes mill ball and powder granule in cylinder be para-curve, and drum rotational speed is 90 rev/mins;
5. open shielding power supply, regulating power makes power on the target unit surface at 4W/cm
2, the beginning sputter coating;
6. after magnetron sputtering 60min, close the power supply of target, stop sputter;
7. close in order under meter, vacuum system, open purging valve and slowly exit in vacuum chamber, after vacuum room pressure and barometric point balance, open vacuum chamber, take out cylinder, mill ball and powder are sieved, obtain the powder of plated film.
Powder after plated film at optical microscope, as shown in Figure 3, can be seen that there is the more uniform copper film of one deck on the surface of solid glass ball powder granule.
Claims (10)
1. facing-target magnetron sputtering system device that is used for the powder granule surface coating is characterized in that: this device comprises the cylinder of vacuum chamber, both ends open, two supporting rolls with spacing inclined-plane, motor and speed regulation device, two magnetron sputtering target holders and shielding power supply;
Wherein, this supporting roll is connected with motor and speed regulation device, the axial level of each supporting roll, is parallel to each other and is positioned at the par height;
This drum shaft is to lying in a horizontal plane on supporting roll, load in cylinder powder granule and/or with the mill ball of the identical material of powder;
These two magnetron sputtering target holders are placed in respectively the both ends open outside of this cylinder, place target on target holder, and axle center and the cylinder of target are axially aligned;
This vacuum chamber is connected with vacuum suction device, and viewing window and purging valve are set on vacuum chamber, and this cylinder, supporting roll and target holder are placed in vacuum chamber.
2. device according to claim 1 is characterized in that: the opening part edge of described cylinder is formed slopely the inclined-plane to the inside, and tilt angle theta is 120～160 degree, the inner diameter d of cylinder opening part
1=d
2/ 3～3d
2/ 4, wherein, d
2Be the cylinder internal diameter.
3. device according to claim 2, it is characterized in that: the length of described supporting roll is identical with drum length, and the angle of inclination on its spacing inclined-plane is identical with the tilt angle theta of the opening part bezel of described cylinder.
4. device according to claim 3, is characterized in that: the outside diameter d of described supporting roll
3=(d
2+ δ)/2～3 (d
2+ δ)/2, δ is the wall thickness of cylinder, the spacing surface width b of supporting roll
1=b
2/ 3～b
2, b
2Surface width for the cylinder opening part.
5. device according to claim 3 is characterized in that: be provided with equably fin on the inwall of described cylinder, and the trend of fin and cylinder axially parallel, the quantity of fin is 4～12, the height h=d of fin
2/ 25～d
2/ 5, the width a=h/6～h of fin.
6. device according to claim 3, it is characterized in that: the distance between described sputter target holder and cylinder opening part is 3cm～20cm.
7. application rights requires the method for the described device of any one to the powder granule surface coating in 1-6, it is characterized in that, comprises the steps:
A. open vacuum chamber, powder granule and mill ball are put into cylinder, cylinder is placed on support roller;
B. required target is arranged on target holder, and is alignd with the axle center of cylinder in the axle center of target;
C. close vacuum chamber, open vacuum suction device, the vacuum of vacuum chamber is extracted into 1 * 10
-4Pa～8 * 10
-3Pa; D. be filled with argon gas to vacuum chamber, control flow with mass flowmeter, when guaranteeing sputter, the vacuum chamber operating air pressure is 0.2Pa～2Pa;
E. open motor, support roller rotarily drives rollers roll, and the rotating speed of regulating electric machine makes mill ball and powder granule in cylinder be para-curve;
F. open shielding power supply, regulating power makes power on the target unit surface at 2W/cm
2～6W/cm
2, the beginning sputter coating;
G. after reaching the thickness of the film that needs sputter, close the power supply of target, stop sputter;
H. close in order under meter, vacuum system, open purging valve and slowly exit in vacuum chamber, after vacuum room pressure and barometric point balance, open vacuum chamber, take out cylinder, mill ball and powder are sieved, obtain the powder of plated film.
8. method according to claim 1, it is characterized in that: the material of described mill ball is identical with the material of powder, perhaps can not pollute powder, and the diameter of mill ball is 3～20mm.
9. method according to claim 8, it is characterized in that: the mass ratio of described powder and mill ball is 0.2～3: 1, and the cumulative volume of powder and mill ball is no more than 45% of cylinder volume.
10. method according to claim 8, it is characterized in that: the speed adjustment scope of cylinder is 0.5～0.96 times of quick passage critical speed, and quick passage critical speed is
Rev/min kind, d
2Be the internal diameter of cylinder, unit is m.
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|---|---|---|---|
| CN2011104275531A CN103160795A (en) | 2011-12-19 | 2011-12-19 | Target magnetron sputtering device and film coating method used for powder particle surface film coating |
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|---|---|---|---|
| CN2011104275531A CN103160795A (en) | 2011-12-19 | 2011-12-19 | Target magnetron sputtering device and film coating method used for powder particle surface film coating |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104480440A (en) * | 2014-11-05 | 2015-04-01 | 烟台首钢磁性材料股份有限公司 | Small size neodymium-iron-boron magnet surface vacuum film plating method and special film plating equipment |
| CN107955937A (en) * | 2016-10-17 | 2018-04-24 | 上海朗亿新材料科技有限公司 | A kind of powder process for dispersing for magnetron sputtering plating |
| CN109735815A (en) * | 2019-01-25 | 2019-05-10 | 浙江野马电池股份有限公司 | Corrosion-inhibiting zinc powder for alkaline manganese battery and preparation process thereof |
| CN110039044A (en) * | 2019-05-29 | 2019-07-23 | 北京金航智造科技有限公司 | A kind of powder surface cladding coating apparatus and method |
| CN113718224A (en) * | 2021-11-01 | 2021-11-30 | 苏州睿锂物联科技有限公司 | Lithium battery cathode material preparation device |
| TWI764732B (en) * | 2019-04-24 | 2022-05-11 | 美商應用材料股份有限公司 | Reactor for coating particles in stationary chamber with rotating paddles |
| CN114481047A (en) * | 2022-01-26 | 2022-05-13 | 广东省新兴激光等离子体技术研究院 | Small-size workpiece coating device, vacuum coating machine and coating method thereof |
| CN114855126A (en) * | 2022-06-02 | 2022-08-05 | 西安稀有金属材料研究院有限公司 | Device and method for modifying surface of micro-nano powder |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113718224A (en) * | 2021-11-01 | 2021-11-30 | 苏州睿锂物联科技有限公司 | Lithium battery cathode material preparation device |
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| CN114481047A (en) * | 2022-01-26 | 2022-05-13 | 广东省新兴激光等离子体技术研究院 | Small-size workpiece coating device, vacuum coating machine and coating method thereof |
| CN114855126A (en) * | 2022-06-02 | 2022-08-05 | 西安稀有金属材料研究院有限公司 | Device and method for modifying surface of micro-nano powder |
| CN114855126B (en) * | 2022-06-02 | 2023-10-27 | 西安稀有金属材料研究院有限公司 | Device and method for modifying surface of micro-nano powder |
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Application publication date: 20130619 |