CN105112874B - The method of the micro-nano film of magnetron sputtering - Google Patents
The method of the micro-nano film of magnetron sputtering Download PDFInfo
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- CN105112874B CN105112874B CN201510615099.0A CN201510615099A CN105112874B CN 105112874 B CN105112874 B CN 105112874B CN 201510615099 A CN201510615099 A CN 201510615099A CN 105112874 B CN105112874 B CN 105112874B
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Abstract
The present invention relates to a kind of method of the micro-nano film of magnetron sputtering, it is characterized in that, include the following steps：（1）Copper wire is wound on the external target on the outside of magnetron sputtering vacuum chamber, the indoor interior target of vacuum chamber and vacuum is cleaned out, matrix is placed on interior target, closing vacuum chamber；（2）To vacuum chamber, vacuum degree 10‑5~10‑6The ratio of Pa, input nitrogen and argon gas filled vacuum room into vacuum chamber, nitrogen and argon gas is 1:3；（3）The current value of copper wire is controlled in 4~13A, and interior target is made to form micro-nano film in matrix surface through magnetron sputtering；First using nickel target to matrix Hong material bombardment 10min, it turns off nickel target and opens chromium target bombardment matrix 3min formation CrN films, it turns off chromium target and opens titanium target bombardment matrix 8min formation TiN films, finally close titanium target opening chromium target bombardment matrix 15min and form Cr CrN composite membranes.The present invention improves magnetron sputtering and biases that indoor biasing ability, ion ionization level reduces the injury to human body in vacuum chamber, improves efficiency during operation.
Description
Technical field
It is especially a kind of that externally-applied magnetic field is increased by electric current the present invention relates to a kind of method of the micro-nano film of magnetron sputtering
Magnetic field intensity optimizes to obtain the method for micro-nano composite membrane.
Background technology
It when magnetron sputtering refers to object with ionic bombardment, is sputtered and disperses out, sputter the object to disperse and be attached to target
Film is made on matrix, sputter phenomenon is formed around attached to as the electrode of fluorescent lamp is sputtered out.Make this
Sputtered film at least needs the substrate of device film and keeps the stage property of vacuum condition（Internal mechanism）, this stage property is
One makes space, and extract the gas in the making space out using vacuum pump.
Often because the deficiency of biasing ability leads to the quantity of the particle bombardment matrix of ionization in magnetron sputtering vacuum chamber
Deficiency, the time sputtered required for making increase, cause in decline and the vacuum chamber of the insufficient composite membrane ability sputtered to matrix
The ionization level of the insufficient nitrogen of magnetic field intensity is insufficient, makes it with chromium ion in matrix for bombarding the decline of the Nitrogen ion concentration of target
On combination degree weaken, so as to cause on matrix micro-nano composite membrane contact angle reduce hydrophobicity decline.
Bias voltage can generally be increased under existence conditions to improve the biasing ability of ion, ionization rate, but increase voltage
It can lead to the shakiness of equipment local voltage, influencing the Percentage bound of ion influences the leakproofness of vacuum chamber, it may appear that chromium ion leaks outside
Target poison ing is caused to human body, there is very big harm.
Invention content
The purpose of the present invention is overcoming the deficiencies in the prior art, a kind of side of the micro-nano film of magnetron sputtering is provided
Method, obtained micro-nano composite membrane have better hydrophobicity, wearability and corrosion resistance.
According to technical solution provided by the invention, the method for the micro-nano film of magnetron sputtering, it is characterized in that, including following
Step：
（1）Copper wire is wound on the external target on the outside of magnetron sputtering vacuum chamber, the indoor interior target of vacuum chamber and vacuum is cleared up
Totally, matrix is placed on interior target, closing vacuum chamber；
（2）To vacuum chamber, vacuum degree 10-5~10-6Pa, nitrogen is inputted into vacuum chamber and argon gas filling is true
The ratio of empty room, nitrogen and argon gas is 1:3；
（3）The current value of copper wire is controlled in 4~13A, and interior target is made to form micro-nano film in matrix surface through magnetron sputtering；
Is turned off by nickel target opening chromium target bombardment matrix 3min and forms CrN films, then close by matrix Hong material bombardment 10min using nickel target first
It closes chromium target and opens titanium target bombardment matrix 8min formation TiN films, finally close titanium target opening chromium target bombardment matrix 15min and form Cr-
CrN composite membranes.
Further, described matrix is the stainless sheet steel after the higher-order of oscillation cleans.
Further, the winding number of turn of the copper wire is 320 circles.
The present invention overcomes existing deficiency, improve magnetron sputtering bias indoor biasing ability, ion in vacuum chamber
Ionization level reduces the injury to human body, improves efficiency during operation.
Description of the drawings
Fig. 1 is the contact angle experiments result of the obtained matrix surface composite membrane of embodiment one under an electron microscope.
Fig. 2 is the contact angle experiments result of the obtained matrix surface composite membrane of embodiment two under an electron microscope.
Fig. 3 is the contact angle experiments result of the obtained matrix surface composite membrane of embodiment three under an electron microscope.
Fig. 4 is the electron microscope of 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 electron microscope of matrix surface composite membrane that comparative example one obtains.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment one：A kind of method of the micro-nano film of magnetron sputtering, includes the following steps：
（1）320 circle copper wires are wound on the external target on the outside of magnetron sputtering vacuum chamber, by the indoor interior target of vacuum chamber and vacuum
It cleans out, matrix is placed on interior target, closing vacuum chamber；Described matrix using after the higher-order of oscillation cleans 25mm ×
The stainless sheet steel of 25mm；
（2）To vacuum chamber, vacuum degree 10-5, nitrogen and argon gas filled vacuum room, nitrogen are inputted into vacuum chamber
Ratio with argon gas is 1:3；
（3）The current value of copper wire is controlled in 4A, and interior target is made to form micro-nano film in matrix surface through magnetron sputtering；First
Using nickel target to matrix Hong material bombardment 10min, turn off nickel target and open chromium target bombardment matrix 3min formation CrN, turn off chromium target
It opens titanium target bombardment matrix 8min and forms TiN, finally it is compound to form Cr-CrN by closing titanium target opening chromium target bombardment matrix 15min
Film.
Embodiment two：A kind of method of the micro-nano film of magnetron sputtering, includes the following steps：
（1）320 circle copper wires are wound on the external target on the outside of magnetron sputtering vacuum chamber, by the indoor interior target of vacuum chamber and vacuum
It cleans out, matrix is placed on interior target, closing vacuum chamber；Described matrix using after the higher-order of oscillation cleans 25mm ×
The stainless sheet steel of 25mm；
（2）To vacuum chamber, vacuum degree 10-6Pa inputs nitrogen and argon gas filled vacuum room, nitrogen into vacuum chamber
The ratio of gas and argon gas is 1:3；
（3）The current value of copper wire is controlled in 13A, and interior target is made to form micro-nano film in matrix surface through magnetron sputtering；It is first
First is turned off by nickel target opening chromium target bombardment matrix 3min and forms CrN, turns off chromium by matrix Hong material bombardment 10min using nickel target
Target opens titanium target bombardment matrix 8min and forms TiN, and finally it is compound to form Cr-CrN by closing titanium target opening chromium target bombardment matrix 15min
Film.
Embodiment three：A kind of method of the micro-nano film of magnetron sputtering, includes the following steps：
（1）320 circle copper wires are wound on the external target on the outside of magnetron sputtering vacuum chamber, by the indoor interior target of vacuum chamber and vacuum
It cleans out, matrix is placed on interior target, closing vacuum chamber；Described matrix using after the higher-order of oscillation cleans 25mm ×
The stainless sheet steel of 25mm；
（2）To vacuum chamber, vacuum degree is 5 × 10-6Pa inputs nitrogen and argon gas filled vacuum into vacuum chamber
The ratio of room, nitrogen and argon gas is 1:3；
（3）The current value of copper wire is controlled in 10A, and interior target is made to form micro-nano film in matrix surface through magnetron sputtering；It is first
First is turned off by nickel target opening chromium target bombardment matrix 3min and forms CrN, turns off chromium by matrix Hong material bombardment 10min using nickel target
Target opens titanium target bombardment matrix 8min and forms TiN, and finally it is compound to form Cr-CrN by closing titanium target opening chromium target bombardment matrix 15min
Film.
Comparative example one：Other conditions are with embodiment three, and electric current is to be worth for 0A on copper wire.
The contact angle of matrix surface composite membrane that measurement embodiment one, embodiment two, embodiment three and comparative example one obtain
Size, the matrix surface contact angle size that one~embodiment of embodiment three obtains is 100o, 97o, 102o, specifically such as Fig. 1~Fig. 3
It is shown, the contact angle experiments knot of the matrix surface composite membrane that respectively one~embodiment of embodiment three obtains under an electron microscope
Fruit, greatly with good wetability and spreadability.Fig. 4 is the obtained electron microscope of matrix surface composite membrane of embodiment three, can be with
See that the micro-nano structure of composite membrane of stainless steel surface is evenly distributed.
Fig. 5 is comparative example one, i.e., when not having externally-applied magnetic field（I.e. in the case of copper wire no power）Obtained stainless steel surface
The surface contact angle size of micro-nano composite membrane, it can be seen that its hydrophobicity is poor.Fig. 6 is the matrix surface that comparative example one obtains
The electron microscope of composite membrane, it can be seen that its micro-nano composite membrane is unevenly distributed.
The present invention passes through the formation of compound plasma injection and settling system on stainless steel material surface layer using electric current
A kind of micro-nano composite membrane adjusts the size increase Cr targets of electric current, the N pole field abilities of the additional solenoid of Ti target Ni targets, increases
The magnetic field intensity of externally-applied magnetic field and non-equilibrium ability promote the ionization level of high pure nitrogen in magnetron sputtering vacuum chamber, pass through Cr targets
Ti target Ni targets bombardment stainless steel surface rises the Forming ability of chromium nitride, the micro-nano composite membrane film base junction for forming stainless steel
Resultant force enhances, surface hydrophobicity ability, wearability, the corrosion resistance of composite membrane.
The present invention, which increases externally-applied magnetic field, increases the bias magnetic field intensity in magnetron sputtering vacuum chamber, stainless steel surface institute shape
Into its contact angle of micro-nano structure of composite membrane（Angle of wetting）Angle increase to 90o ~ 107o, the micro-nano structure of composite membrane of formation
The hydrophobic ability enhancing on surface.
Claims (1)
1. a kind of method of the micro-nano film of magnetron sputtering, it is characterized in that, include the following steps：
（1）Copper wire is wound on the external target on the outside of magnetron sputtering vacuum chamber, the indoor interior target of vacuum chamber and vacuum is cleaned out,
Matrix is placed on interior target, closing vacuum chamber；
（2）To vacuum chamber, vacuum degree 10-5~10-6Pa inputs nitrogen and argon gas filled vacuum room into vacuum chamber,
The ratio of nitrogen and argon gas is 1:3；
（3）The current value of copper wire is controlled in 4~13A, and interior target is made to form micro-nano film in matrix surface through magnetron sputtering；First
Using nickel target to matrix Hong material bombardment 10min, turn off nickel target and open chromium target bombardment matrix 3min, turn off chromium target and open titanium target
Matrix 8min is bombarded, titanium target is finally closed and opens chromium target bombardment matrix 15min；Described matrix be after the higher-order of oscillation cleans not
Become rusty steel sheet；The winding number of turn of the copper wire is 320 circles.
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| CN201510615099.0A CN105112874B (en) | 2015-09-24 | 2015-09-24 | The method of the micro-nano film of magnetron sputtering |
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| JP2003231962A (en) * | 2002-02-13 | 2003-08-19 | National Institute Of Advanced Industrial & Technology | Process for manufacturing metal, alloy or ceramic molded product with highly hard surface |
| SG143940A1 (en) * | 2003-12-19 | 2008-07-29 | Agency Science Tech & Res | 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. |