CN105112874A - Micro/nano film magnetic-control sputtering method - Google Patents
Micro/nano film magnetic-control sputtering method Download PDFInfo
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- CN105112874A CN105112874A CN201510615099.0A CN201510615099A CN105112874A CN 105112874 A CN105112874 A CN 105112874A CN 201510615099 A CN201510615099 A CN 201510615099A CN 105112874 A CN105112874 A CN 105112874A
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Abstract
The invention relates to a micro/nano film magnetic-control sputtering method. The micro/nano film magnetic-control sputtering method comprises the following steps of (1) winding copper wires on an outer target on the outer side of a magnetic-control sputtering vacuum chamber, thoroughly cleaning the vacuum chamber and an inner target of the vacuum chamber, placing a matrix on the inner target and closing the vacuum chamber; (2) vacuumizing the vacuum chamber until the vacuum degree is 10-5-10-6Pa, and filling nitrogen and argon in the vacuum chamber under the condition that the ratio of the nitrogen to the argon is 1:3; and (3) controlling a current value of the copper wires at 4-13A, performing magnetic-control sputtering of the inner target on the surface of the matrix to form a micro/nano film, performing bombardment on a bombardment material of the matrix for 10 minutes by using a nickel target, closing the nickel target, and opening a chrome target to perform bombardment on the matrix for 15 minutes to form a Cr-CrN composite film. By the micro/nano film magnetic-control sputtering method, eccentric compression capability in a magnetic-control sputtering eccentric compression chamber and ionization of ions in the vacuum chamber are improved, injury to human bodies is reduced, and operation efficiency is improved.
Description
Technical field
The present invention relates to the method for the micro-nano film of a kind of magnetron sputtering, especially a kind of magneticstrength optimization by electric current increase externally-applied magnetic field obtains the method for micro-nano composite membrane.
Background technology
When magnetron sputtering refers to object with ionic bombardment, sputtered disperse out, sputter the object dispersed and be attached in target substrate and make film, the electrode as fluorescent lamp be sputtered out and attached work in around form sputter phenomenon.Make this sputtered film, at least need the substrate of device film and keep the stage property (internal mechanism) of vacuum condition, this stage property is a making space, and uses vacuum pump to be extracted out by the gas in this making space.
Often because the deficiency of biasing ability causes the quantity not sufficient of the particle bombardment matrix ionized in magnetron sputtering vacuum chamber, the time of required sputtering is increased, cause the decline of not enough composite membrane ability of matrix sputtering and the ionization level of the not enough nitrogen of vacuum chamber internal magnetic field intensity is not enough, itself and the chromium ion combination degree on matrix can be weakened for the Nitrogen ion density loss of bombardment target, thus cause the micro-nano composite membrane contact angle on matrix to reduce hydrophobicity declining.
Bias voltage generally can be increased to improve biasing ability, the specific ionization of ion under existence conditions, but increase the shakiness that voltage can cause equipment local voltage, the combination rate affecting ion affects the stopping property of vacuum chamber, there will be chromium ion and leaks outside and cause target poison ing to human body, have very large harm.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide the method for the micro-nano film of a kind of magnetron sputtering, the micro-nano composite membrane obtained has better hydrophobicity, wear resistance and corrosion resistance.
According to technical scheme provided by the invention, the method for the micro-nano film of described magnetron sputtering, is characterized in that, comprise the following steps:
(1) external target outside magnetron sputtering vacuum chamber is wound around copper wire, target in vacuum chamber and vacuum chamber is cleaned out, matrix is placed on interior target, closing vacuum chamber;
(2) to vacuum chamber, vacuum tightness is 10
-5~ 10
-6pa, inputs nitrogen and argon gas filled vacuum room in vacuum chamber, and the ratio of nitrogen and argon gas is 1:3;
(3) control the current value of copper wire at 4 ~ 13A, and make interior target form micro-nano film through magnetron sputtering at matrix surface; First adopt nickel target to matrix Hong material bombardment 10min, close nickel target again and open chromium target bombardment matrix 3min formation CrN film, close chromium target again and open titanium target bombardment matrix 8min formation TiN film, finally close titanium target and open chromium target bombardment matrix 15min formation Cr-CrN composite membrane.
Further, described matrix is the stainless steel sheet after HF oscillation cleaning.
Further, the winding number of turn of described copper wire is 320 circles.
Instant invention overcomes existing deficiency, improve ion ionization level in the biasing ability of magnetron sputtering bias voltage indoor, vacuum chamber and reduce the injury to human body, improve efficiency during operation.
Accompanying drawing explanation
Fig. 1 is the matrix surface composite membrane contact angle experiments result under an electron microscope that embodiment one obtains.
Fig. 2 is the matrix surface composite membrane contact angle experiments result under an electron microscope that embodiment two obtains.
Fig. 3 is the matrix surface composite membrane contact angle experiments result under an electron microscope that embodiment three obtains.
Fig. 4 is the Electronic Speculum figure of the matrix surface composite membrane that embodiment three obtains.
Fig. 5 is the surface contact angle experimental result of the micro-nano composite membrane of stainless steel surface that comparative example one obtains.
Fig. 6 is the Electronic Speculum figure of the matrix surface composite membrane that comparative example one obtains.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment one: the method for the micro-nano film of a kind of magnetron sputtering, comprises the following steps:
(1) external target outside magnetron sputtering vacuum chamber is wound around 320 circle copper wires, target in vacuum chamber and vacuum chamber is cleaned out, matrix is placed on interior target, closing vacuum chamber; Described matrix adopts the stainless steel sheet of the 25mm × 25mm after HF oscillation cleaning;
(2) to vacuum chamber, vacuum tightness is 10
-5, in vacuum chamber, input nitrogen and argon gas filled vacuum room, the ratio of nitrogen and argon gas is 1:3;
(3) control the current value of copper wire at 4A, and make interior target form micro-nano film through magnetron sputtering at matrix surface; First adopt nickel target to matrix Hong material bombardment 10min, then close nickel target and open chromium target bombardment matrix 3min and form CrN, then close chromium target and open titanium target bombardment matrix 8min and form TiN, finally close titanium target and open chromium target bombardment matrix 15min and form Cr-CrN composite membrane.
Embodiment two: the method for the micro-nano film of a kind of magnetron sputtering, comprises the following steps:
(1) external target outside magnetron sputtering vacuum chamber is wound around 320 circle copper wires, target in vacuum chamber and vacuum chamber is cleaned out, matrix is placed on interior target, closing vacuum chamber; Described matrix adopts the stainless steel sheet of the 25mm × 25mm after HF oscillation cleaning;
(2) to vacuum chamber, vacuum tightness is 10
-6pa, inputs nitrogen and argon gas filled vacuum room in vacuum chamber, and the ratio of nitrogen and argon gas is 1:3;
(3) control the current value of copper wire at 13A, and make interior target form micro-nano film through magnetron sputtering at matrix surface; First adopt nickel target to matrix Hong material bombardment 10min, then close nickel target and open chromium target bombardment matrix 3min and form CrN, then close chromium target and open titanium target bombardment matrix 8min and form TiN, finally close titanium target and open chromium target bombardment matrix 15min and form Cr-CrN composite membrane.
Embodiment three: the method for the micro-nano film of a kind of magnetron sputtering, comprises the following steps:
(1) external target outside magnetron sputtering vacuum chamber is wound around 320 circle copper wires, target in vacuum chamber and vacuum chamber is cleaned out, matrix is placed on interior target, closing vacuum chamber; Described matrix adopts the stainless steel sheet of the 25mm × 25mm after HF oscillation cleaning;
(2) to vacuum chamber, vacuum tightness is 5 × 10
-6pa, inputs nitrogen and argon gas filled vacuum room in vacuum chamber, and the ratio of nitrogen and argon gas is 1:3;
(3) control the current value of copper wire at 10A, and make interior target form micro-nano film through magnetron sputtering at matrix surface; First adopt nickel target to matrix Hong material bombardment 10min, then close nickel target and open chromium target bombardment matrix 3min and form CrN, then close chromium target and open titanium target bombardment matrix 8min and form TiN, finally close titanium target and open chromium target bombardment matrix 15min and form Cr-CrN composite membrane.
Comparative example one: other condition is with embodiment three, and on copper wire, electric current take value as 0A.
Measure the contact angle size of the matrix surface composite membrane that embodiment one, embodiment two, embodiment three and comparative example one obtain, the matrix surface contact angle size that embodiment one ~ embodiment three obtains is 100o, 97o, 102o, specifically as shown in FIG. 1 to 3, be respectively the matrix surface composite membrane contact angle experiments result under an electron microscope that embodiment one ~ embodiment three obtains, there is greatly good wettability and spreadability.Fig. 4 is the Electronic Speculum figure of the matrix surface composite membrane that embodiment three obtains, and can see that the micro-nano structure of composite membrane of stainless steel surface is evenly distributed.
Fig. 5 is comparative example one, and namely the surface contact angle size of the micro-nano composite membrane of stainless steel surface that (in copper cash no power situation) obtains when not having externally-applied magnetic field, can find out that its hydrophobicity is poor.Fig. 6 is the Electronic Speculum figure of the matrix surface composite membrane that comparative example one obtains, and can see its micro-nano composite membrane skewness.
The present invention utilize electric current by compound plasma inject and settling system at the micro-nano composite membrane of the one of the formation on stainless material top layer, the size of electric current is regulated to increase Cr target, the N pole field ability of the additional solenoid of Ti target Ni target, increase the magneticstrength of externally-applied magnetic field and non-equilibrium ability, promote the ionization level of high pure nitrogen in magnetron sputtering vacuum chamber, the Forming ability of chromium nitride is made to increase by Cr target Ti target Ni target bombardment stainless steel surface, the micro-nano composite membrane film-substrate cohesion that stainless steel is formed strengthens, the surface hydrophobicity ability of composite membrane, wear resistance, erosion resistance.
The present invention increases externally-applied magnetic field makes the bias voltage magneticstrength in magnetron sputtering vacuum chamber increase, stainless steel surface form its contact angle of micro-nano structure of composite membrane (wetting angle) angle increase to 90o ~ 107o, the hydrophobic ability on the micro-nano structure of composite membrane surface of formation strengthens.
Claims (3)
1. a method for the micro-nano film of magnetron sputtering, is characterized in that, comprise the following steps:
(1) external target outside magnetron sputtering vacuum chamber is wound around copper wire, target in vacuum chamber and vacuum chamber is cleaned out, matrix is placed on interior target, closing vacuum chamber;
(2) to vacuum chamber, vacuum tightness is 10
-5~ 10
-6pa, inputs nitrogen and argon gas filled vacuum room in vacuum chamber, and the ratio of nitrogen and argon gas is 1:3;
(3) control the current value of copper wire at 4 ~ 13A, and make interior target form micro-nano film through magnetron sputtering at matrix surface; First adopt nickel target to matrix Hong material bombardment 10min, then close nickel target and open chromium target bombardment matrix 3min, then close chromium target and open titanium target bombardment matrix 8min, finally close titanium target and open chromium target bombardment matrix 15min.
2. the method for the micro-nano film of magnetron sputtering as claimed in claim 1, is characterized in that: described matrix is the stainless steel sheet after HF oscillation cleaning.
3. the method for the micro-nano film of magnetron sputtering as claimed in claim 1, is characterized in that: the winding number of turn of described copper wire is 320 circles.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030150713A1 (en) * | 2002-02-13 | 2003-08-14 | National Institute Of Advanced Industrial Science And Technology | Method of forming a surface coating having high surface hardness on a metal, alloy or ceramic substrate |
| US20050136656A1 (en) * | 2003-12-19 | 2005-06-23 | Zeng Xian T. | Process for depositing composite coating on a surface |
| CN101876062A (en) * | 2009-11-10 | 2010-11-03 | 武汉大学 | Hollow cathode sputtering ion plating device |
| CN102453878A (en) * | 2010-10-27 | 2012-05-16 | 鸿富锦精密工业（深圳）有限公司 | Coating device |
-
2015
- 2015-09-24 CN CN201510615099.0A patent/CN105112874B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030150713A1 (en) * | 2002-02-13 | 2003-08-14 | National Institute Of Advanced Industrial Science And Technology | Method of forming a surface coating having high surface hardness on a metal, alloy or ceramic substrate |
| US20050136656A1 (en) * | 2003-12-19 | 2005-06-23 | Zeng Xian T. | Process for depositing composite coating on a surface |
| CN101876062A (en) * | 2009-11-10 | 2010-11-03 | 武汉大学 | Hollow cathode sputtering ion plating device |
| CN102453878A (en) * | 2010-10-27 | 2012-05-16 | 鸿富锦精密工业（深圳）有限公司 | Coating device |
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Address after: 214199 Donggang Town, Xishan District, Wuxi City, Jiangsu Province Patentee after: Jiangsu ZOJE Seiko Polytron Technologies Inc Address before: 214199 Lipo Industrial Park, Donggang Town, Xishan District, Wuxi City, Jiangsu Province Patentee before: Wuxi Zhongjie Vibration Isolators Co., Ltd. |