CN204529950U - A kind of wear-resisting dewatering nano laminated film - Google Patents
A kind of wear-resisting dewatering nano laminated film Download PDFInfo
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- CN204529950U CN204529950U CN201520130804.3U CN201520130804U CN204529950U CN 204529950 U CN204529950 U CN 204529950U CN 201520130804 U CN201520130804 U CN 201520130804U CN 204529950 U CN204529950 U CN 204529950U
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Abstract
一种耐磨疏水纳米复合薄膜，属于金属表面处理和改性技术领域。该复合薄膜是以高速钢、或钛合金、或硬质合金、或纯金属为基体，在其表面依次制备有纯金属薄膜、带有微结构形貌的纳米复合薄膜。制备方法为首先利用电弧离子镀在基体材料表面沉积一层力学性能优异的纳米复合硬质薄膜，然后再利用超快激光加工技术在薄膜表面产生微纳双重结构，制备成了兼具优良力学性能和一定疏水性能的表面薄膜。本实用新型制备的薄膜保留了纳米复合硬质薄膜优良的力学性能：表面硬度高、韧性、耐磨性、抗划伤性能强，通过构造薄膜表面的微结构形貌使薄膜具备了一定的疏水性能。该制备方法设备相对简单、成本低、能耗低、无污染，能够实现高效的绿色制造。
The invention discloses a wear-resistant and hydrophobic nano-composite film, which belongs to the technical field of metal surface treatment and modification. The composite film is based on high-speed steel, or titanium alloy, or hard alloy, or pure metal, on the surface of which a pure metal film and a nanocomposite film with microstructure morphology are sequentially prepared. The preparation method is to first deposit a layer of nanocomposite hard film with excellent mechanical properties on the surface of the base material by arc ion plating, and then use ultrafast laser processing technology to produce a micro-nano double structure on the surface of the film to prepare a composite with excellent mechanical properties. And a surface film with certain hydrophobic properties. The film prepared by the utility model retains the excellent mechanical properties of the nanocomposite hard film: high surface hardness, toughness, wear resistance, and strong scratch resistance, and the film has a certain degree of hydrophobicity by constructing the microstructure of the film surface performance. The preparation method has relatively simple equipment, low cost, low energy consumption and no pollution, and can realize efficient green manufacturing.
Description
Technical field
The invention belongs to metal finishing and technical field of modification, particularly the wear-resisting dewatering nano laminated film of one.
Background technology
Along with the fast development of modern manufacturing industry and the constantly complicated of material military service environment, utilize ganoine thin film to carry out important channel that surface modification becomes material surface protection gradually, simultaneously also proposes more and more higher requirement to the use properties of ganoine thin film.Under a lot of harsh usage environment, in the fields such as the marine anticorrosion of anti-icing, the naval vessel surface metal of such as carrier-borne aircraft engine intake, require that ganoine thin film has stronger over-all properties, excellent mechanical property to be had on the one hand, to improve component surface wear resistant friction reducing characteristic, also need good hydrophobicity on the other hand, play and strengthen anti-icing and moisture-proof role.Therefore, the ganoine thin film seeking to have excellent mechanical performance and high hydrophobicity becomes an important channel of improving material surface protection.
It is generally acknowledged, the superhydrophobic characteristic of material surface is caused jointly by solid surface energy and surface fine structure.In recent years, along with the discovery of biological surface lotus leaf effect, research about micro-structure surface ultra-hydrophobicity becomes focus, the hydrophobic fundamental research of various biological surface is shown, many biological surfaces have the hierarchical structure that micron is combined with nanophase, the bilayer that this micro-nano-scale combines or the complicated coarse structure of multilayer just many biological surfaces have the basic reason of ultra-hydrophobicity, people inspire by this, by the such as ultrafast laser processing of application surface micro-processing technology, ultraviolet photolithographic, plasma etching, the technology such as electron beam lithography achieve the ultra-hydrophobicity of material surface at the complicated coarse structure that material surface making micro-nano-scale combines, self-cleaning characteristic material being had be unsurpassed in excellence, material anti-pollution, anti-aging, anti-oxidation, the ability such as anticorrosive is also greatly enhanced.
At present, the research for hydrophobic film mainly concentrates on organic polymer film and Nanocomposites functional membrane, wherein, in the research of organic polymer thin film, although hydrophobic performance is improved significantly, is still faced with following problem:
(1) mechanical property of organic polymer thin film itself is not high, and surface hardness is lower, toughness, wear resistance are poor, and resistance to marring can reach requirement.Hardness as fluorine carbon hydrophobic film only has 2 ~ 3GPa.
(2) film-substrate cohesion of organic polymer thin film is lower, and flushing resistance is poor.The bonding force obtained as fluorine carbon hydrophobic film scratch experiment is lower than 10N.
(3) source material prepared needed for organic polymer thin film mostly is expensive fluorocarbon gas, and part is even poisonous, not only causes environmental pollution, also can affect personnel safety.
Therefore, how to possess durable microtexture and the higher thin-film material of physical strength is the key point and the difficult point that build weather resistance hydrophobic film simultaneously.
The present invention is intended to, on the basis ensureing mechanical property, pursue hydrophobic performance as much as possible, to widen the range of application of ganoine thin film.
Utility model content
In order to solve the problems referred to above that prior art exists, the invention provides a kind of wear-resisting dewatering nano laminated film and preparation method thereof.The nano combined ganoine thin film being characterized in first utilizing arc ions to be plated in substrate material surface deposits a kind of excellent in mechanical performance, and then utilize ultrafast laser processing technology to produce micro-nano dual structure at film surface.
Hydrophobicity is caused jointly by solid surface energy and surface fine structure, although nano compound film mostly is nitrogen (carbon) compound of covalent linkage, belong to high surface energy material, and Herminghaus proposes, the surface that any material can be made to form with the surface of mechanism of stratum becomes not wettable, means that on high surface energy material, construct hierarchical structure also can obtain hydrophobic surface.
The technical scheme that the present invention is adopted for achieving the above object is: a kind of wear-resisting dewatering nano laminated film, it is characterized in that, described laminated film be with rapid steel or titanium alloy or Wimet or pure metal for matrix, prepare successively on its surface and have pure metal film, nano compound film with microstructure appearance.
The wear-resisting dewatering nano laminated film of described one, is characterized in that: the thickness of described pure metal film is 0.05 ~ 0.2 μm, and the thickness of the described nano compound film with microstructure appearance is 0.8 ~ 1.0 μm.
The wear-resisting dewatering nano laminated film of described one, is characterized in that: it is greater than 140 ° to the contact angle of water.
The preparation method of described a kind of wear-resisting dewatering nano laminated film, is characterized in that, the method comprises following concrete sequential steps:
(1) metal works cleaning
Metal works is placed in filtered cathode vacuum arc equipment through cleaning, drying, passes into argon gas under vacuum and carry out the cleaning of argon ion aura;
(2) thin film deposition
Surface of workpiece after step (1) process deposits one deck pure metal film; After completing, continue the nano combined ganoine thin film of deposition one deck at surface of workpiece; Cooling down is to room temperature afterwards, takes out metal works;
(3) ultrafast laser processing
The metal works of the nano combined ganoine thin film of described surface deposition one deck is placed on the work top of laser micro-processing equipment, open laser apparatus, laser beam scan path is set, carry out laser processing, make the nano combined ganoine thin film of surface of workpiece produce micro-nano dual structure, prepare the nano compound film with microstructure appearance.
The preparation method of described a kind of wear-resisting dewatering nano laminated film, is characterized in that: the material of described metal works is the one in rapid steel, titanium alloy, Wimet, pure metal.
The preparation method of described a kind of wear-resisting dewatering nano laminated film, is characterized in that: in described step (1), passes into before argon gas carries out aura cleaning and background air pressure must be made lower than 5 × 10
-3pa; Air pressure in aura cleaning process should maintain 0.1Pa ~ 3Pa, and the negative pulse bias voltage that substrate applies is set to-1000V ~ 0, and dutycycle is 10% ~ 90%, and operating frequency is 5KHz ~ 45KHz, and the time is 0 ~ 20min.
The preparation method of described a kind of wear-resisting dewatering nano laminated film, it is characterized in that: in described step (2), in membrane-film preparation process, pass into argon gas and nitrogen, keep deposition pressure between 0.1Pa ~ 1Pa, the depositing time of pure metal film is 10mins ~ 20mins, and the depositing time of nano combined ganoine thin film is 60mins ~ 120mins.
The preparation method of described a kind of wear-resisting dewatering nano laminated film, is characterized in that: in described step (3), and the laser micro-processing equipment of application is picosecond laser micro Process equipment; The micro-nano dual structure prepared on nano combined ganoine thin film surface is array square column microstructure, and the width of array square column is 10 ~ 500 μm, and the degree of depth of array square column is 10 ~ 100 μm; Laser scanning region forms the micro-nano secondary structure of papillary, and mastoid process diameter is 1 ~ 10 μm.
The wear-resisting dewatering nano laminated film of one of the present utility model, initiative utilize arc ion plating (aip) and ultrafast laser processing technology have prepared the Nanocrystalline Composite Films with microstructure appearance at workpiece surface, have excellent mechanical property and good hydrophobicity concurrently, the beneficial effect that can bring is:
(1) mechanical property of film itself is excellent, remain the relevant mechanical property of nano combined ganoine thin film, surface hardness is high, toughness, wear resistance, adhesion strength be strong, hardness is higher than 40GPa, frictional coefficient, lower than 0.4, can be applied under the usage environment of harshness;
(2) film-substrate cohesion of film is high, is greater than 70N, effectively extends the work-ing life of workpiece;
(3) while the mechanical property ensureing film excellence, have good hydrophobic performance, water contact angle is greater than 140 °;
(4) this preparation method's equipment used is relatively simple, and cost is low, and energy consumption is low, pollution-free, can realize efficient green manufacturing.
Accompanying drawing explanation
Fig. 1 is the cross sectional profile views of a kind of wear-resisting dewatering nano laminated film of the present invention and metallic matrix thereof.
In figure, 1. pure metal film, 2. with the nano compound film of microstructure appearance.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, but the present invention is not limited to specific embodiment.
Embodiment 1
A preparation method for wear-resisting dewatering nano laminated film, comprises following concrete sequential steps:
(1) workpiece cleaning
Rapid steel workpiece, before loading vacuum chamber, adopts the cleaning that MVWH5-3045 type charing water element cleaning machine carries out, successively through the cleaning of ultrasonic wave water, the displacement of pure water ultrasonic cleaning, water, negative pressure of vacuum ultrasonic cleaning, reduced steam cleaning-drying.This cleaning introduces vacuum cleaned and vacuum-drying integrated technique scheme on the basis of conventional ultrasound water cleaning, avoids cleaning and dry separation and the secondary pollution introduced; Replace conventional organic solvents to carbonize water element, have and clean feature thoroughly; In addition, continuous and automatic cleaning process is adopted, significant increase cleaning efficiency.
Thin film deposition experiment strengthens on Magnetic filter pulsed bias arc ion plating equipment in MMLab-Arc-II type and carries out.First mechanical pump, lobe pump and molecular pump is adopted to bleed to vacuum chamber, when base vacuum is lower than 5 × 10
-3during Pa, rapid steel workpiece carries out the argon ion aura cleaning of 10min, to remove passive film and other impurity of rapid steel workpiece surface.Design parameter in aura cleaning process is: air pressure is 0.1Pa, and the negative pulse bias voltage amplitude that rapid steel workpiece applies is-1000V, and dutycycle is 10%, and frequency is 5KHz.
(2) thin film deposition
In membrane-film preparation process, pass into Ar gas and N
2gas, maintenance deposition pressure is 0.1Pa, lights cathode targets form plasma body by high-voltage pulse, under the effect of workpiece negative bias, then accelerates to arrive workpiece surface finally form rete.For improving the homogeneity of film, sample table planetary rotation.
First deposit one deck pure metal film 1 at rapid steel workpiece surface, depositing time is 10mins; After completing, continue the nano combined ganoine thin film of deposition one deck at rapid steel workpiece surface, depositing time is 60mins; Be reduced to room temperature cooling afterwards, take out metal works;
(3) ultrafast laser processing
To be placed on the work top of laser micro-processing equipment after the rapid steel workpiece ultrasonic cleaning of the nano combined ganoine thin film of described surface deposition one deck, open laser apparatus, laser beam scan path is set, carries out laser processing.The single beam laser that picosecond laser produces by optical component and condenser lens directly by laser focusing at sample surfaces, fixed laser, by computer programming, the structure that different sample motion tracks realizes different cycles micro-nano structure is set, the micro-nano dual structure prepared on nano combined ganoine thin film surface is array square column microstructure, the width of array square column is 10 μm, and the degree of depth of array square column is 10 μm; Laser scanning region forms the micro-nano secondary structure of papillary, and mastoid process diameter is 1 μm.Make the nano combined ganoine thin film of rapid steel workpiece surface produce micro-nano dual structure, prepare the nano compound film 2 with microstructure appearance.
So melt at rapid steel workpiece surface and cover the wear-resisting dewatering nano laminated film of one deck, record the film-substrate cohesion 85N of film, hardness 42GPa, frictional coefficient is 0.33, and water contact angle is 142 °.
Embodiment 2
The preparation method of described wear-resisting dewatering nano laminated film, is characterized in that, the method comprises following concrete sequential steps:
(1) workpiece cleaning
Titanium alloy workpiece, before loading vacuum chamber, adopts the cleaning that MVWH5-3045 type charing water element cleaning machine carries out, successively through the cleaning of ultrasonic wave water, the displacement of pure water ultrasonic cleaning, water, negative pressure of vacuum ultrasonic cleaning, reduced steam cleaning-drying.This cleaning introduces vacuum cleaned and vacuum-drying integrated technique scheme on the basis of conventional ultrasound water cleaning, avoids cleaning and dry separation and the secondary pollution introduced; Replace conventional organic solvents to carbonize water element, have and clean feature thoroughly; In addition, continuous and automatic cleaning process is adopted, significant increase cleaning efficiency.
Thin film deposition experiment strengthens on Magnetic filter pulsed bias arc ion plating equipment in MMLab-Arc-II type and carries out.First mechanical pump, lobe pump and molecular pump is adopted to bleed to vacuum chamber, when base vacuum is lower than 5 × 10
-3during Pa, all workpiece carry out the argon ion aura cleaning of 5min, to remove passive film and other impurity on titanium alloy workpiece surface.Design parameter in aura cleaning process is: air pressure is 1.5Pa, and the negative pulse bias voltage amplitude that titanium alloy workpiece applies is-500V, and dutycycle is 50%, and frequency is 25KHz.
(2) thin film deposition
In membrane-film preparation process, pass into Ar gas and N
2gas, maintenance deposition pressure is 0.5Pa, lights cathode targets form plasma body by high-voltage pulse, under the effect of titanium alloy workpiece negative bias, then accelerates to arrive workpiece surface finally form rete.For improving the homogeneity of film, sample table planetary rotation.
First at titanium alloy workpiece surface deposition one deck pure metal film 1, depositing time is 15mins; After completing, continue the nano combined ganoine thin film of deposition one deck on titanium alloy workpiece surface, depositing time is 90mins; Be reduced to room temperature cooling afterwards, take out titanium alloy workpiece;
(3) ultrafast laser processing
To be placed on the work top of laser micro-processing equipment after the titanium alloy workpiece ultrasonic cleaning of the nano combined ganoine thin film of described surface deposition one deck, open laser apparatus, laser beam scan path is set, carries out laser processing.The single beam laser that picosecond laser produces by optical component and condenser lens directly by laser focusing at sample surfaces, fixed laser, by computer programming, the structure that different sample motion tracks realizes different cycles micro-nano structure is set, the micro-nano dual structure prepared on nano combined ganoine thin film surface is array square column microstructure, the width of array square column is 250 μm, and the degree of depth of array square column is 55 μm; Laser scanning region forms the micro-nano secondary structure of papillary, and mastoid process diameter is 5 μm.Make the nano combined ganoine thin film of surface of workpiece produce micro-nano dual structure, prepare the nano compound film 2 with microstructure appearance.
So melt on titanium alloy workpiece surface and cover the wear-resisting dewatering nano laminated film of one deck, record the film-substrate cohesion 72N of film, hardness 43GPa, frictional coefficient is 0.38, and water contact angle is 141 °.
Embodiment 3
The preparation method of described wear-resisting dewatering nano laminated film, is characterized in that, the method comprises following concrete sequential steps:
(1) workpiece cleaning
Hard alloy workpiece, before loading vacuum chamber, adopts the cleaning that MVWH5-3045 type charing water element cleaning machine carries out, successively through the cleaning of ultrasonic wave water, the displacement of pure water ultrasonic cleaning, water, negative pressure of vacuum ultrasonic cleaning, reduced steam cleaning-drying.This cleaning introduces vacuum cleaned and vacuum-drying integrated technique scheme on the basis of conventional ultrasound water cleaning, avoids cleaning and dry separation and the secondary pollution introduced; Replace conventional organic solvents to carbonize water element, have and clean feature thoroughly; In addition, continuous and automatic cleaning process is adopted, significant increase cleaning efficiency.
Thin film deposition experiment strengthens on Magnetic filter pulsed bias arc ion plating equipment in MMLab-Arc-II type and carries out.First mechanical pump, lobe pump and molecular pump is adopted to bleed to vacuum chamber, when base vacuum is lower than 5 × 10
-3during Pa, all workpiece carry out the argon ion aura cleaning of 20min, to remove passive film and other impurity of workpiece surface.Design parameter in aura cleaning process is: air pressure is 3Pa, and the negative pulse bias voltage amplitude that workpiece applies is-200V, and dutycycle is 90%, and frequency is 45KHz.
(2) thin film deposition
In membrane-film preparation process, pass into Ar gas and N
2gas, maintenance deposition pressure is 1Pa, lights cathode targets form plasma body by high-voltage pulse, under the effect of workpiece negative bias, then accelerates to arrive workpiece surface finally form rete.For improving the homogeneity of film, sample table planetary rotation.
First at hard alloy workpiece surface deposition one deck pure metal film 1, depositing time is 20mins; After completing, continue the nano combined ganoine thin film of deposition one deck on hard alloy workpiece surface, depositing time is 120mins; Be reduced to room temperature cooling afterwards, take out hard alloy workpiece;
(3) ultrafast laser processing
To be placed on the work top of laser micro-processing equipment after the hard alloy workpiece ultrasonic cleaning of the nano combined ganoine thin film of described surface deposition one deck, open laser apparatus, laser beam scan path is set, carries out laser processing.The single beam laser that picosecond laser produces by optical component and condenser lens directly by laser focusing at sample surfaces, fixed laser, by computer programming, the structure that different sample motion tracks realizes different cycles micro-nano structure is set, the micro-nano dual structure prepared on nano combined ganoine thin film surface is array square column microstructure, the width of array square column is 500 μm, and the degree of depth of array square column is 100 μm; Laser scanning region forms the micro-nano secondary structure of papillary, and mastoid process diameter is 10 μm.Make the nano combined ganoine thin film on hard alloy workpiece surface produce micro-nano dual structure, prepare the nano compound film 2 with microstructure appearance.
So melt on hard alloy workpiece surface and cover the wear-resisting dewatering nano laminated film of one deck, record the film-substrate cohesion 71N of film, hardness 46GPa, frictional coefficient is 0.37, and water contact angle is 144 °.
Embodiment 4
The preparation method of described wear-resisting dewatering nano laminated film, is characterized in that, the method comprises following concrete sequential steps:
(1) workpiece cleaning
Pure metal workpiece, before loading vacuum chamber, adopts the cleaning that MVWH5-3045 type charing water element cleaning machine carries out, successively through the cleaning of ultrasonic wave water, the displacement of pure water ultrasonic cleaning, water, negative pressure of vacuum ultrasonic cleaning, reduced steam cleaning-drying.This cleaning introduces vacuum cleaned and vacuum-drying integrated technique scheme on the basis of conventional ultrasound water cleaning, avoids cleaning and dry separation and the secondary pollution introduced; Replace conventional organic solvents to carbonize water element, have and clean feature thoroughly; In addition, continuous and automatic cleaning process is adopted, significant increase cleaning efficiency.
(2) thin film deposition
In membrane-film preparation process, pass into Ar gas and N
2gas, maintenance deposition pressure is 0.3Pa, lights cathode targets form plasma body by high-voltage pulse, under the effect of workpiece negative bias, then accelerates to arrive workpiece surface finally form rete.For improving the homogeneity of film, sample table planetary rotation.
First deposit one deck pure metal film 1 at pure metal workpiece surface, depositing time is 20mins; After completing, continue the nano combined ganoine thin film of deposition one deck at pure metal workpiece surface, depositing time is 60mins; Be reduced to room temperature cooling afterwards, take out pure metal workpiece;
(3) ultrafast laser processing
To be placed on the work top of laser micro-processing equipment after the pure metal workpiece ultrasonic cleaning of the nano combined ganoine thin film of described surface deposition one deck, open laser apparatus, laser beam scan path is set, carries out laser processing.The single beam laser that picosecond laser produces by optical component and condenser lens directly by laser focusing at sample surfaces, fixed laser, by computer programming, the structure that different sample motion tracks realizes different cycles micro-nano structure is set, the micro-nano dual structure prepared on nano combined ganoine thin film surface is array square column microstructure, the width of array square column is 300 μm, and the degree of depth of array square column is 70 μm; Laser scanning region forms the micro-nano secondary structure of papillary, and mastoid process diameter is 7 μm.Make the nano combined ganoine thin film of pure metal workpiece surface produce micro-nano dual structure, prepare the nano compound film 2 with microstructure appearance.
So melt at pure metal workpiece surface and cover the wear-resisting dewatering nano laminated film of one deck, record the film-substrate cohesion 74N of film, hardness 44GPa, frictional coefficient is 0.35, and water contact angle is 142 °.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694877A (en) * | 2015-03-06 | 2015-06-10 | 常州翊迈新材料科技有限公司 | Wear-resistant hydrophobic nano composite film and preparation method thereof |
| CN109161851A (en) * | 2018-07-28 | 2019-01-08 | 华中科技大学 | A kind of preparation method and product in the super hydrophilic pet sheet face based on induced with laser |
-
2015
- 2015-03-06 CN CN201520130804.3U patent/CN204529950U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694877A (en) * | 2015-03-06 | 2015-06-10 | 常州翊迈新材料科技有限公司 | Wear-resistant hydrophobic nano composite film and preparation method thereof |
| CN109161851A (en) * | 2018-07-28 | 2019-01-08 | 华中科技大学 | A kind of preparation method and product in the super hydrophilic pet sheet face based on induced with laser |
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