CN201665704U - Ultrasonic specimen stage applied to magnetron sputtering coating of powder - Google Patents
Ultrasonic specimen stage applied to magnetron sputtering coating of powder Download PDFInfo
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- CN201665704U CN201665704U CN2010201328294U CN201020132829U CN201665704U CN 201665704 U CN201665704 U CN 201665704U CN 2010201328294 U CN2010201328294 U CN 2010201328294U CN 201020132829 U CN201020132829 U CN 201020132829U CN 201665704 U CN201665704 U CN 201665704U
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- ultrasonic
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- syntonizer
- sampling receptacle
- magnetron sputtering
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Abstract
The utility model discloses an ultrasonic specimen stage applied to magnetron sputtering coating of powder, which comprises a specimen container, a resonator and an ultrasonic generator, the specimen container is positioned above the resonator, and the resonator is connected with the ultrasonic generator through a cable. In the process of magnetron sputtering coating of powder, an ultrasonic frequency of 20kHz-500kHz and power of 50W-2000W are adjusted to drive the resonator, then the resonator can exert sound waves on the specimen container evenly, so the powder in the specimen container can flop up and down and be dispersed evenly, and an even film can be coated on the surface of the powder, then the purpose of even magnetron sputtering coating of powder can be achieved.
Description
Technical field
The utility model relates to the sample table device that a kind of vacuum plating is used, and more particularly says, is meant a kind of ultrasonic sample table that is used for the powder granule magnetron sputtering plating.
Background technology
Powder granule is little owing to particle diameter, specific surface area greatly has block materials and do not had various physics and chemical property, therefore, at present both at home and abroad the various characteristics of the powder granule of multiple series and the research of application have been obtained bigger progress, but relevant method and application facet thereof at the powder granule surface coating still done positive exploration, and one of difficulty that needs solution is the homodisperse problem of powder granule.
Method at the powder granule surface coating is a lot, as vacuum-evaporation, magnetron sputtering, electroless plating, chemical vapour deposition and sol-gel method etc.Magnetron sputtered deposition technology wherein owing to the sputtering raste height, advantages such as the substrate temperature rise is low, film-the Ji bonding force is good, device performance is stable, convenient operation and control are subjected to increasing application.
The patent No. is to disclose a kind of " technology of vacuum metal film plating on microparticle surface and equipment thereof " among the ZL 200510014639.6, and this equipment comprises vacuum chamber, sputter target holder, specimen holder, sample table, well heater, vacuum suction device, purging valve, viewing window and vibration machine.This equipment claimed is rotated with vibration effect simultaneously just can make the powder homodisperse.
Summary of the invention
A kind of ultrasonic sample table that is used for powder magnetic control sputtering coating of the utility model design, this ultrasonic sample table includes sampling receptacle, syntonizer and ultrasonic generator, sampling receptacle places the syntonizer top, and syntonizer links to each other with ultrasonic generator by cable.Syntonizer is set below sampling receptacle, this syntonizer can be applied to the sound wave that ultrasonic generator produces on the sampling receptacle equably, because the wall thickness of sampling receptacle is thinner, therefore sound wave is applied in the powder in the sampling receptacle equably, and powder presents bob and reaches homodisperse under the effect of sound wave.In the magnetron sputtering membrane process, the bob of powder fully exposes powder surface, and this helps forming metallic membrane at powder surface.Drive syntonizer by ultrasonic frequency and the power of regulating ultrasonic generator output,, also can allow the interior powder of sampling receptacle disperse equably even this syntonizer can guarantee to use the ultra-large type sampling receptacle also can realize the uniform distribution of sound wave.
The utility model adopts ultrasonic sample table to carry out powder magnetic control sputtering coating and includes the following step:
(A) open vacuum chamber, the sampling receptacle that powder body material is housed is installed in the top of syntonizer;
(B) close vacuum chamber, the mechanical pump of opening in the vacuum suction device is evacuated to 0.7Pa～0.9Pa;
(C) molecular pump of opening in the vacuum suction device is evacuated to 2.0 * 10
-3Pa～5.0 * 10
-3Pa;
(D) open under meter, applying argon gas is to 0.3Pa～0.4Pa in vacuum chamber;
(E) open ultrasonic generator, regulate ultrasonic frequency 20kHz～500kHz and power 50W～2000W;
(F) open target power supply, regulate power, the beginning sputter coating to 500W～1500W;
(G) close target power supply behind 100min～600min, stop sputter.
(H) close under meter, molecular pump and mechanical pump in order, open purging valve again and slowly exit in vacuum chamber, after vacuum room pressure and barometric point balance, open vacuum chamber, take out sampling receptacle, plated film finishes.
Description of drawings
Fig. 1 is a magnetron sputtering film device synoptic diagram.
Fig. 2 is the structure iron of the utility model ultrasonic sample table.
Fig. 3 is a ultrasonic sample table exploded view of the present utility model.
Fig. 4 is another visual angle structure iron of the utility model sampling receptacle.
Fig. 5 is electron scanning micrograph and the X-ray energy spectrum figure of cenosphere before and after plated film.
Fig. 6 is an electron scanning micrograph before and after the plated film of SiC particle under different amplification.
Fig. 7 is the X-ray diffractogram of SiC particle before and after plated film.
Among the figure: 1. vacuum chamber 2. sputter target holders 3. specimen holders 4. sample table 4A. ultrasonic generators 41. sampling receptacles 411. cavitys 412. bottoms 413. threaded holes, 42. syntonizers, 422. cables, 423. threaded post, 6. vacuum suction devices, 7. viewing windows, 8. purging valves
Embodiment
Below in conjunction with drawings and Examples the utility model is described in further detail.
A kind of magnetron sputtering film device referring to shown in Figure 1 includes vacuum chamber 1, sputter target holder 2, specimen holder 3, sample table 4, ultrasonic generator 4A, vacuum suction device 6, viewing window 7 and purging valve 8; Vacuum chamber 1 internal upper part is provided with sputter target holder 2, and its underpart correspondence is provided with specimen holder 3, is provided with sample table 4 above the specimen holder 3, also is provided with viewing window 7, purging valve 8 on the vacuum chamber 1, and vacuum suction device 6 is by pipeline and vacuum chamber 1 UNICOM; And corresponding connection traffic meter, molecular pump and mechanical pump, dispose electrical equipment control and cooling circulating water system simultaneously.Distance between sputter target holder 2 and the sample table 4 is designated as h, h=5cm～30cm.
In the utility model, in order to solve powder granule homodisperse problem in the magnetron sputtering membrane process, utility model people has solved this problem by the improvement to sample table 4.By a syntonizer 42 is set below sampling receptacle 41, syntonizer 42 is connected with the ultrasonic generator 4A of vacuum chamber 1 outside, in coating process, drive syntonizer 42 formation vibrations by frequency and the power of adjusting ultrasonic generator 4A output, and then make the powder granule bob in the sampling receptacle 41 also disperse equably, realized uniform film on the powder surface plating better.
Include sampling receptacle 41, syntonizer 42 and ultrasonic generator 4A referring to Fig. 2, Fig. 3, sample table 4 shown in Figure 4, sampling receptacle 41 places syntonizer 42 tops, and syntonizer 42 links to each other with ultrasonic generator 4A by cable 422.Sampling receptacle 41 is provided with cavity 411, and this cavity 411 is used to place material to be processed (powder body material); The centre of the bottom 412 of sampling receptacle 41 is provided with threaded hole 413, and this threaded hole 413 is installed in syntonizer 42 tops with the thread fit realization of threaded post 423 with sampling receptacle 41.Sampling receptacle 41 adopts metal material processing, and its wall thickness is 0.2mm～1.0mm.A threaded post 423 is installed in the improvement of syntonizer 42 above syntonizer 42, this threaded post 423 is installed in the threaded hole 413 of sampling receptacle 41 bottoms.Syntonizer 42 is set below sampling receptacle 41, it can be applied to the inside and outside equally distributed sound wave of ring the bottom 412 of sampling receptacle 41 equably, because the diapire of sampling receptacle 41 is thinner, syntonizer 42 can be applied to the inside and outside equally distributed sound wave of ring in the powder in the sample table equably, so equally distributed sound wave energy makes the powder bob in the sample table and disperses equably under the diapire.Drive syntonizer 42 by ultrasonic frequency and the power of regulating ultrasonic generator 4A output, even this toroidal resonator 42 can guarantee to use ultra-large type sampling receptacle 41 also can realize the uniform distribution of sound wave, also can allow sampling receptacle 41 interior powders disperse equably.
The equipment of the utility model design can carry out magnetron sputtering plating to micro particulate materials, and this micro particulate materials can be inorganic materials, organic materials and biomaterial etc.; Shape can also be that hollow, porous or other are various irregularly shaped except that regular shapes such as sphere; Sputtering target material mainly comprises metallic substance such as silver, copper, aluminium, cobalt and nickel, also can be other non-metallic material and organic materials.
The utility model design in the magnetron sputtering membrane process, auxiliary bob mode is disperseed powder body material, prepared microparticle surface metal film has the following advantages: (1) is by regulating output frequency and the power of ultrasonic generator 4A, with and being used in combination of the device 42 that shakes together, make each microparticle in the sampling receptacle 41 all have an opportunity fully to expose its surface, therefore utilize ultrasonic wave aid magnetron sputtering method institute metal-coated films to have the advantage of good uniformity, compactness height and strong adhesion; (2) processing condition such as vibrational frequency by changing operating air pressure, sputtering power, temperature, sputtering time and syntonizer 42 in the vacuum chamber and target just can be at the various metallic films of microparticle surface deposition of different shape; (3) preceding at filling with inert gas in vacuum chamber (as argon gas), the residual gas pressure in the control vacuum chamber utilizes this method institute metal-coated films purity to significantly improve; (4) this method has advantages such as simple, no waste water and gas pollution of technical process and water-saving and electricity-saving.
To be example at coal fly ash hollow micro bead surface magnetic control sputtering metallizing copper film, its processing step is as follows:
(A) open vacuum chamber 1, the sampling receptacle 41 of the coal fly ash hollow micro bead of packing into is installed in going up (threaded post 423 on the syntonizer 42 cooperates with the threaded hole 413 of sampling receptacle 41 bottoms) of syntonizer 42;
(B) close vacuum chamber 1, the mechanical pump of opening in the vacuum suction device 6 is evacuated to 0.8Pa;
(C) molecular pump of opening in the vacuum suction device 6 is evacuated to 2.5 * 10
-3Pa;
(D) open under meter, applying argon gas is to 0.4Pa in vacuum chamber 1;
(E) open ultrasonic generator 4A, regulate ultrasonic frequency 20kHz and power 1000W;
(F) open target power supply, regulate power, beginning sputter copper plating film to 1000W; Target is that purity reaches 99.99% circular copper target;
(G) close target power supply behind the 300min, stop sputter.
(H) close under meter, molecular pump and mechanical pump in order, open slowly venting in vacuum chamber 1 of purging valve 8 again, after vacuum chamber 1 internal pressure and barometric point balance, open vacuum chamber 1, take out sampling receptacle 41, plated film finishes.
Fig. 5 is electron scanning micrograph and the X-ray energy spectrum figure of cenosphere before and after plated film.(a) and (c) be plated film cenosphere not; (b) and (d) be cenosphere copper coating film; (a) and (b) be electron scanning micrograph; (c) and (d) be X-ray energy spectrum figure.As can be seen, uncoated cenosphere surface is very smooth from accompanying drawing (a), and any metallic particles is not almost found on the surface; The surface of cenosphere also exists white point, this be since when scanning electronic microscope detects the electric charge of hollow bead surface accumulate and to cause, illustrate that the electroconductibility on plated film cenosphere surface is not very poor.As can be seen, the cenosphere particle surface that is coated with copper film is obviously rough from accompanying drawing 2 (b), has many metallic particles to exist.From the X-ray energy spectrometer photo of accompanying drawing 2 (c) and 2 (d) as can be seen, cenosphere has only the characteristic peak of O, Si and Al before the plated film, and the cenosphere that is coated with copper film is except O, Si and Al, the characteristic peak that also has Cu, more than explanation cenosphere surface successfully on the plating metal copper film.
To be example at SiC particle surface magnetron sputtering nickel plating film, its processing step is as follows:
(A) open vacuum chamber 1, the SiC particulate sampling receptacle 41 of packing into is installed in going up (threaded post 423 on the syntonizer 42 cooperates with the threaded hole 413 of sampling receptacle 41 bottoms) of syntonizer 42;
(B) close vacuum chamber 1, the mechanical pump of opening in the vacuum suction device 6 is evacuated to 0.9Pa;
(C) molecular pump of opening in the vacuum suction device 6 is evacuated to 3.2 * 10
-3Pa;
(D) open under meter, applying argon gas is to 0.4Pa in vacuum chamber 1;
(E) open ultrasonic generator 4A, regulate ultrasonic frequency 40kHz and power 600W;
(F) open target power supply, regulate power, beginning sputter plated nickel film to 1200W; Target is that purity reaches 99.99% circular nickel target;
(G) close target power supply behind the 240min, stop sputter.
(H) close under meter, molecular pump and mechanical pump in order, open slowly venting in vacuum chamber 1 of purging valve 8 again, after vacuum chamber 1 internal pressure and barometric point balance, open vacuum chamber 1, take out sampling receptacle 41, plated film finishes.
Fig. 6 is an electron scanning micrograph before and after the plated film of SiC particle under different amplification: (a) and (c) be plated film SiC not; (b) and (d) be coated with the SiC of metallic nickel film for the surface; (a) and (b) for amplifying 5000 times electron scanning micrograph; (c) and (d) for amplifying 10000 times electron scanning micrograph.As can be seen, the SiC particle is very smooth at the plated film front surface, is difficult to find that the SiC surface exists small-particle; And through behind the plated film, silicon carbide obviously exists a lot of molecules, and SiC surface plating upper film is described.
The X-ray diffractogram that Fig. 7 is the SiC particle before and after plated film: (a) be plated film SiC not; (b) plated nickel film SiC.Can find out that from accompanying drawing 4 (a) the SiC particle crystallization before the plated film is fine, but the diffraction peak of SiC only occur; And in accompanying drawing 4 (b), diffracting spectrum is except the diffraction peak that SiC occurred, diffraction peak has also appearred in the position that at 2 θ angles is 44.5 °, 51.6 ° and 76.2 °, respectively with JADE-SCAN software in (111) of standard powder x-ray diffraction card 65-0380 pure metal Ni, (200) and (220) crystal face are corresponding.Can judge thus, the SiC surface successfully on the plating metallic nickel film, and prepared nickel film is a face-centred cubic structure.
Claims (3)
1. ultrasonic sample table that is applicable to that powder magnetic control sputtering coating is used, it is characterized in that: this ultrasonic sample table includes sampling receptacle, syntonizer and ultrasonic generator, sampling receptacle places the syntonizer top, and syntonizer links to each other with ultrasonic generator by cable.
2. the ultrasonic sample table that is applicable to that powder magnetic control sputtering coating is used according to claim 1 is characterized in that: sampling receptacle adopts metal material processing, and its wall thickness is 0.2mm～1.0mm.
3. the ultrasonic sample table that is applicable to that powder magnetic control sputtering coating is used according to claim 1 is characterized in that: the ultrasonic frequency of ultrasonic generator output is that 20kHz～500kHz and output rating are 50W～2000W.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010201328294U CN201665704U (en) | 2010-03-16 | 2010-03-16 | Ultrasonic specimen stage applied to magnetron sputtering coating of powder |
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|---|---|---|---|
| CN2010201328294U CN201665704U (en) | 2010-03-16 | 2010-03-16 | Ultrasonic specimen stage applied to magnetron sputtering coating of powder |
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| CN201665704U true CN201665704U (en) | 2010-12-08 |
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| CN2010201328294U Expired - Fee Related CN201665704U (en) | 2010-03-16 | 2010-03-16 | Ultrasonic specimen stage applied to magnetron sputtering coating of powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798677A (en) * | 2010-03-16 | 2010-08-11 | 北京航空航天大学 | Ultrasonic sample table and method for carrying out powder magnetic control sputtering coating by using same |
| CN107022743A (en) * | 2016-02-01 | 2017-08-08 | 上海朗亿功能材料有限公司 | A kind of magnetic-control sputtering continuous plating equipment for micro-nano powder |
| CN109207946A (en) * | 2018-09-12 | 2019-01-15 | 杭州联芳科技有限公司 | A kind of nick-eltitanium alloy stent surface treatment method |
-
2010
- 2010-03-16 CN CN2010201328294U patent/CN201665704U/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798677A (en) * | 2010-03-16 | 2010-08-11 | 北京航空航天大学 | Ultrasonic sample table and method for carrying out powder magnetic control sputtering coating by using same |
| CN101798677B (en) * | 2010-03-16 | 2012-01-11 | 北京航空航天大学 | Ultrasonic sample table and method for carrying out powder magnetic control sputtering coating by using same |
| CN107022743A (en) * | 2016-02-01 | 2017-08-08 | 上海朗亿功能材料有限公司 | A kind of magnetic-control sputtering continuous plating equipment for micro-nano powder |
| CN107022743B (en) * | 2016-02-01 | 2019-04-02 | 上海朗亿功能材料有限公司 | A kind of magnetic-control sputtering continuous plating equipment for micro-nano powder |
| CN109207946A (en) * | 2018-09-12 | 2019-01-15 | 杭州联芳科技有限公司 | A kind of nick-eltitanium alloy stent surface treatment method |
| CN109207946B (en) * | 2018-09-12 | 2022-05-20 | 杭州联芳科技有限公司 | Nickel-titanium alloy stent surface treatment method |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101208 Termination date: 20130316 |