CN105543781A - Device for vacuum coating of magnetic powder particle surfaces and coating method - Google Patents
Device for vacuum coating of magnetic powder particle surfaces and coating method Download PDFInfo
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- CN105543781A CN105543781A CN201510978378.3A CN201510978378A CN105543781A CN 105543781 A CN105543781 A CN 105543781A CN 201510978378 A CN201510978378 A CN 201510978378A CN 105543781 A CN105543781 A CN 105543781A
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- Prior art keywords
- vacuum
- magnetic powder
- magnet coil
- sample table
- vacuum chamber
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Classifications
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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
- C23C14/24—Vacuum 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
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
-
- 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
- C23C14/351—Sputtering by application of a magnetic field, e.g. magnetron sputtering using a magnetic field in close vicinity to the substrate
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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
The invention aims at providing a device for vacuum coating of magnetic powder particle surfaces and a coating method. According to the device and the coating method provided by the invention, by using the response of magnetic powder particles to an alternating magnetic field, the magnetic powder particles can generate changes of lifting (stacking), falling, turning (rotating) and the like in a vacuum chamber, so that uniform vacuum coating of the magnetic powder particles in a vacuum environment can be realized. According to the device and the coating method provided by the invention, the vacuum chamber is produced by using austenitic stainless steel; and the change of the alternating magnetic field is controlled by adopting a relay, so that the aim of uniformly and compactly coating the magnetic powder particles is achieved.
Description
Technical field
The present invention relates to a kind of magnetic powder particle surface technique for vacuum coating, comprise the technique for vacuum coating such as evaporation, magnetron sputtering, be applied particularly to the fields such as environmental protection, pharmacy, material.
Background technology
Magnetic powder surface coating or modification, all have a wide range of applications in various fields such as environment protection, biomedicine, stealthy technique and Physics of Magnetism.The method of particle surface plated film or modification mainly contains liquid phase method and vapor phase process.
The severe reaction conditions of liquid phase method, poor repeatability.Adopt the chemical process plated films such as plating, electroless plating, sol-gel, due to the reason of interfacial chemistry, the film formed is uneven, purity is low, compactness is poor, the surface film material formed sometimes is difficult to the problem reaching surface modification, the material system of superficial film also can be restricted, and is also easy to cause the pollution to environment simultaneously.
Gas phase rule has good conformality, particularly physical vacuum coating technology, and reaction conditions is gentle, has repetitive operation relatively preferably.The magnet rotor of existing magnetic stirring particles stirs, powder sheds method, powder vibratory drilling method, supersonic method, vacuum atomizing suspends, gas holder method, can stir uneven due to the reunion of magnetic-particle, in scattering mechanism, regional area powder is lower by the probability shed, have the powder of significant proportion by shake to surface probability compared with low, expression area is little, the vacuum tightness of air the reason such as to be lowered and to cause plated film uneven, not fine and close.Because magnetic powder has magnetic, have agglomeration each other, cause the degree of difficulty of plated film to increase, plated film homogeneity reduces, and even filming equipment cannot use.Meanwhile, in physical vacuum film coating method, the plated film of vacuum evaporation and magnetron sputtering has certain directivity, even if therefore particle is suspended in the air, is also difficult to plated film even.
Summary of the invention
The object of the invention is, for magnetic powder particle, to overcome the defect of prior art, propose to utilize magnetic field force to carry out the apparatus and method of vacuum uniform coated to magnetic powder particle.Present method in the environment that vacuum tightness is extremely low, can carry out vacuum plating to magnetic powder particle, can produce plated film evenly, the functional materials of strong adhesion.The method can adopt the vacuum coating technology such as vacuum evaporation, magnetron sputtering, and can carry out the plated film of multiple material to particle surface simultaneously, and production process is environment friendly and pollution-free.
For achieving the above object, the present invention includes following technical scheme:
A kind of for magnetic powder particle surface vacuum coater, this device comprises vacuum chamber, magnet coil or magnetic field of volution coil, high temperature resistant special-shaped crucible, sputtering target holder, shielding power supply, evaporation power supply, sample table, supporting roll, rly., AC power; Wherein, magnet coil can be positioned at the top (as Fig. 1) of device, and also can be positioned at sample table (as Fig. 3) surrounding of vacuum chamber, now sample table is cup-shaped.Magnetic field in Fig. 2 can be set to rotatingfield; According to the needs of vacuum plating, can be symmetrical arranged multiple special-shaped high-temperature crucible and magnetron sputtering target holder, the two can be arranged separately also can combine setting, and when combination is arranged, its mutual alignment, cross section as depicted in figs. 1 and 2; Vacuum chamber is connected with vacuum suction device, vacuum chamber is arranged viewing window and purging valve.
Device as above, wherein, vacuum chamber material adopts austenitic stainless steel (304).
Device as above, in Fig. 1, magnet coil is unshakable in one's determination around cylindricality, to strengthen the magneticstrength produced, and be vertically in the top of sample table, the medullary ray of magnet coil and the medullary ray of sample table coincide at vertical direction, and magnet coil horizontal projection is within the horizontal projection scope of sample table.
Device as above, wherein, the power acquisition 220V of magnet coil or rotatingfield coil, 50Hz alternating-current, alternating-current is connected with rly., and the opening time of rly. is 0.5 ~ 3 second.
Device as above, wherein, magnet coil adopts high-temperature resistant enamelled wire, and the high temperature resistant number of degrees are for being more than or equal to 200 degrees Celsius.
Device as above, wherein, the external diameter of magnet coil is 0.50 ~ 0.90mm.
Device as above, in Fig. 1, special-shaped crucible peripheral tangent line AB, DE respectively with the top edge point C of sample table and bottom margin point E point-blank.
Device as above, in Fig. 2, sample table is barrel-shaped, upper opening, and chassis is arranged at bottom.
Device as above, in Fig. 2, has rotatingfield coil or the magnet coil of interchange around sample table.
On the other hand, the present invention includes application device as described below to the method for magnetic powder particle surface plated film, performing step is as follows:
A. open vacuum chamber, magnetic powder particle is placed in sample table;
If B. need adopt magnetron sputtering, be then arranged on target holder by required target, target can select target of the same race, also can select target not of the same race;
If C. need adopt vacuum plating, then the material of required evaporation is put into high temperature resistant special-shaped crucible according to the order of design, deposition material can select same material, also can select not same material;
D. close vacuum chamber, open vacuum suction device, the vacuum in vacuum chamber is extracted into 1 × 10
-4pa ~ 6 × 10
-3pa;
E. according to magnetron sputtering plating mode, then need to pour argon gas to vacuum chamber, ensure that vacuum chamber operating pressure is 0.5Pa ~ 1.5Pa;
F. open the power supply of magnet coil, under the effect of rly., magnetic powder particle can produce the motion such as lift-off, landing, upset (as shown in Figure 1 device), or produce be piled into post, fall, the phenomenon (as shown in Figure 2 device) such as rotation;
G. open vacuum evaporation power supply or shielding power supply, carry out plated film by design requirements at magnetic powder particle surface;
H. after reaching the thickness needing plated film, close vacuum plating power supply or vacuum plating power supply, stop plated film, close the power supply of magnet coil;
I. close vacuum system, open purging valve slowly to vacuum chamber venting, after pressure and the barometric point of vacuum indoor balances, open vacuum chamber, taking-up magnetic powder, then the uniform powder of acquisition plated film.
Method as above, wherein, when in coating process due to reasons such as the risings of gas temperature in vacuum chamber, cause the plated film of magnetic powder particle uneven, the mode of batch-plating can be adopted, namely first close vacuum evaporation power supply or shielding power supply, until magnetic powder particle after temperature reduces recovery magnetic, then carry out plated film.
Method as above, in Fig. 1 device, if the magneticstrength that the magnetic of magnetic powder particle is not enough or magnet coil produces is powerful not, then can regulate the height of sample table, to adjust the distance between magnet coil and magnetic powder particle, alternating magnetic field is made to produce larger effect to magnetic powder particle and carry out plated film.
The invention has the beneficial effects as follows: the measure of control that this device adopts alternating magnetic field to change as magnetic powder particle motion, the vacuum tightness in vacuum plating process can be reduced in, and magnetic powder particle can be made can to produce continuous print lift-off (piling up), fall, overturn mode of motion such as (rotations), be beneficial to uniform coated under vacuum state, utilize the surface modifying material that the method is produced, there is plated film even compact, the feature that bonding force is strong.
In sum, apparatus structure of the present invention is simple, easy to operate, controls precisely.
Accompanying drawing explanation
Fig. 1 is the structural representation for magnetic powder particle surface vacuum coater of the present invention.
Fig. 2 is the structural representation of another mode for magnetic powder particle surface vacuum coater of the present invention.
Fig. 3 is the sectional position figure of high temperature resistant special-shaped crucible and sputtering target material in Fig. 1 or Fig. 2.
Fig. 4 is rotatingfield coil schematic diagram in Fig. 2.
In figure, 1-rly., 2-vacuum chamber, 3-sample table, 4-supporting roll, 5-ordinary stainless steel plate, 6-magnet coil, 7-flute profile blank flange (austenitic stainless steel), 8-flange, 9-is high temperature resistant special-shaped crucible, 10-viewing window, 11-cathode sputtering target, 12-pumped vacuum systems, 13-rotatingfield coil or magnet coil.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
As depicted in figs. 1 and 2 for magnetic powder particle surface vacuum coater and film coating method, it is characterized in that vacuum chamber 2 material adopts austenitic stainless steel (304) to make, magnetic powder particle is placed in sample table 3, by pumped vacuum systems 12, vacuum chamber is made to form vacuum environment, now, magnet coil 6 or rotating coil 13 pass into alternating-current, under the effect of rly. 1, form the alternating magnetic field cut in and out, magnetic powder particle then under the effect of alternating magnetic field, can produce lift-off (piling up), falls, overturns modes such as (rotations).
Further, high temperature resistant special-shaped crucible 9 and magnetic control spattering target frame 11 is provided with, when carrying out vacuum plating to magnetic powder, now in vacuum chamber 2, high temperature resistant special-shaped crucible 9 can be filled with Coating Materials of the same race or not of the same race, and target frame 11 also can install target of the same race or not of the same race; High temperature resistant special-shaped crucible 9 and magnetic control spattering target frame 11, carry out the need of filling deposition material or target as required when plated film; When magnetic powder aloft with in sample table carry out going up to the air (piling up), fall, overturn dynamic changes such as (rotations) time, open evaporation power supply or radio-frequency power supply, vacuum plating carried out to magnetic powder particle surface.
With regard to magnetic powder, can not rely on and the vacuum tightness in vacuum chamber, and under Absolute truth reciprocal of duty cycle state, carry out plated film, simultaneously in the process of plated film, magnetic powder constantly can carry out going up to the air (piling up), fall, overturn the change of states such as (rotations) under the effect of alternating magnetic field, thus the probability making the every bit on powder granule surface be exposed in air is identical, probability towards the direction of evaporation or magnetron sputtering is the same, thus can obtain the magnetic powder particle that plated film is even, fine and close.
Specific embodiment is as follows:
A. open vacuum chamber, a certain amount of magnetic powder particle is put into sample table, required vacuum coating material is put into high temperature resistant special-shaped crucible, required target is arranged on target holder;
B. close vacuum chamber, open vacuum suction device, the vacuum of vacuum chamber is extracted into 0.4 × 10
-3pa;
If C. plated film needs magnetron sputtering, then in vacuum chamber, be filled with argon gas, control flow with mass flowmeter, when ensureing to sputter, vacuum work air pressure is 0.6Pa; Carry out vacuum evaporation if only need, then do not need to be filled with argon gas in vacuum chamber;
D. open the AC power of magnet coil (Fig. 1) or rotatingfield coil (Fig. 2), rly. works simultaneously, and magnetic powder particle is carried out going up to the air (piling up), fall, overturn the change of kinestates such as (rotations);
E. open evaporation power supply or shielding power supply, carry out vacuum plating;
F., after vacuum plating for some time, evaporation power supply or shielding power supply is closed;
If be G. necessary, also after evaporation power supply or shielding power supply close for some time, can restart, carry out batch-plating;
H. close under meter, vacuum system successively, open purging valve and slowly exit in vacuum chamber, after vacuum indoor pressure and barometric point balance, open vacuum chamber, take out the magnetic powder particle of plated film.
Claims (10)
1. the apparatus and method for magnetic powder surface vacuum coating, it is characterized in that: this device comprises vacuum chamber, magnet coil or rotatingfield coil, high temperature resistant special-shaped crucible, magnetron sputtering target holder, shielding power supply, evaporation power supply, sample table (liftable), supporting roll, rly., AC power, wherein, magnet coil can be positioned at the top (as Fig. 1) of vacuum outdoor location, also can be positioned at (as Fig. 2) surrounding of the sample table of vacuum chamber, now basal disc is cup-shaped.
2. the magnetic field in Fig. 2 can add as rotatingfield, and corresponding is rotatingfield coil, and rotatingfield coil as shown in Figure 4; According to the needs of vacuum plating, can arrange special-shaped high-temperature crucible and the magnetron sputtering target holder of multiple symmetry, the two jointly can arrange and also can arrange separately, if jointly arrange, its plane mutual alignment as shown in Figure 3; Vacuum chamber is connected with vacuum suction device, vacuum chamber is arranged viewing window and purging valve.
3. device according to claim 1, is characterized in that: vacuum chamber material adopts austenitic stainless steel (304) or do not have magnetic and withstand voltage material formation.
4. device according to claim 1, it is characterized in that: in Fig. 1, magnet coil is arranged around cylindricality iron core, to strengthen the magneticstrength produced, and be vertically in the top of sample table, the medullary ray of magnet coil and the medullary ray of sample table coincide at vertical direction, and magnet coil horizontal projection is within the horizontal projection of sample table.
5. device according to claim 1, is characterized in that: in Fig. 1 and Fig. 2, the power acquisition 220V of magnet coil, 50Hz alternating-current, and alternating-current is connected with rly., and the opening time of rly. was set between 0.5 ~ 3 second.
6. device according to claim 1, is characterized in that: magnet coil adopts high-temperature resistant enamelled wire, and the high temperature resistant number of degrees are for being more than or equal to 200 degrees Celsius; Device according to claim 1, is characterized in that: the external diameter of magnet coil is 0.50 ~ 0.90mm.
7. device according to claim 1, is characterized in that: in Fig. 1, special-shaped crucible peripheral tangent line AB, DE respectively with the top edge point C of sample table and bottom margin point E point-blank.
8. device according to claim 1, is characterized in that: in Fig. 2, sample table is barrel-shaped, upper opening, and chassis is arranged at bottom.
9. device according to claim 1, is characterized in that: Fig. 2 kind, has magnet coil or rotatingfield coil around sample table.
10. device according to claim 1, is characterized in that, comprises following magnetic powder particle surface vacuum plating mode:
Fig. 1 is in a vacuum, open magnet coil, under the effect of rly., magnetic powder particle (not losing magnetism in certain temperature range) constantly will go up to the air in the certain spatial dimension along with the change of alternating magnetic field in vacuum chamber, land, upset etc., now, vacuum evaporation or magnetron sputtering plating is carried out;
Fig. 2 is in a vacuum, open magnet coil, under the effect of rly., magnetic powder particle (not losing magnetism in certain temperature range) will make response along with the change in magnetic field, magnetic powder particle flies up under the influence of a magnetic field, rotate, to fall etc. the change of state, thus the object of uniform coated can be reached, when magnetic powder has good magnetic in plated film state, continuous coating or batch-plating can be adopted, when magnetic powder at high temperature loses magnetism or magnetic is more weak, adopt batch-plating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510978378.3A CN105543781A (en) | 2015-12-23 | 2015-12-23 | Device for vacuum coating of magnetic powder particle surfaces and coating method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510978378.3A CN105543781A (en) | 2015-12-23 | 2015-12-23 | Device for vacuum coating of magnetic powder particle surfaces and coating method |
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|---|---|
| CN105543781A true CN105543781A (en) | 2016-05-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510978378.3A Pending CN105543781A (en) | 2015-12-23 | 2015-12-23 | Device for vacuum coating of magnetic powder particle surfaces and coating method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517420A (en) * | 2016-11-22 | 2017-03-22 | 兰州交通大学 | Construction method for magnetic film for water purification and magnetic film filtering device |
| CN106517421A (en) * | 2016-11-27 | 2017-03-22 | 兰州交通大学 | Construction method for hydraulic suspension magnetic membrane used for water purification, and magnetic membrane filtration apparatus |
| CN107064833A (en) * | 2017-04-18 | 2017-08-18 | 蔡立汉 | A kind of easy gyromagnet set tester |
| CN109504946A (en) * | 2018-12-20 | 2019-03-22 | 兰州空间技术物理研究所 | A kind of planar rectangular magnetic control sputtering cathode adjustable angle type electromagnetic coil |
| CN111575654A (en) * | 2020-05-21 | 2020-08-25 | 南京航空航天大学 | Ultrasonic vibration assisted vacuum micro-evaporation plating equipment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004152687A (en) * | 2002-10-31 | 2004-05-27 | Sekisui Chem Co Ltd | Manufacturing device and manufacturing method of conductive particulate |
| CN103436848A (en) * | 2013-08-15 | 2013-12-11 | 蚌埠玻璃工业设计研究院 | Vacuum atomization suspension uniform sputtering coating method for spherical powder material |
-
2015
- 2015-12-23 CN CN201510978378.3A patent/CN105543781A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004152687A (en) * | 2002-10-31 | 2004-05-27 | Sekisui Chem Co Ltd | Manufacturing device and manufacturing method of conductive particulate |
| CN103436848A (en) * | 2013-08-15 | 2013-12-11 | 蚌埠玻璃工业设计研究院 | Vacuum atomization suspension uniform sputtering coating method for spherical powder material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517420A (en) * | 2016-11-22 | 2017-03-22 | 兰州交通大学 | Construction method for magnetic film for water purification and magnetic film filtering device |
| CN106517421A (en) * | 2016-11-27 | 2017-03-22 | 兰州交通大学 | Construction method for hydraulic suspension magnetic membrane used for water purification, and magnetic membrane filtration apparatus |
| CN107064833A (en) * | 2017-04-18 | 2017-08-18 | 蔡立汉 | A kind of easy gyromagnet set tester |
| CN109504946A (en) * | 2018-12-20 | 2019-03-22 | 兰州空间技术物理研究所 | A kind of planar rectangular magnetic control sputtering cathode adjustable angle type electromagnetic coil |
| CN109504946B (en) * | 2018-12-20 | 2020-12-01 | 兰州空间技术物理研究所 | Angle-adjustable electromagnetic coil for planar rectangular magnetron sputtering cathode |
| CN111575654A (en) * | 2020-05-21 | 2020-08-25 | 南京航空航天大学 | Ultrasonic vibration assisted vacuum micro-evaporation plating equipment |
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