CN101962769A - Method for preparing hydrophobic film on surface of material - Google Patents
Method for preparing hydrophobic film on surface of material Download PDFInfo
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- CN101962769A CN101962769A CN 201010299440 CN201010299440A CN101962769A CN 101962769 A CN101962769 A CN 101962769A CN 201010299440 CN201010299440 CN 201010299440 CN 201010299440 A CN201010299440 A CN 201010299440A CN 101962769 A CN101962769 A CN 101962769A
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Abstract
The invention belongs to the technical field of material surface modification, and relates to the improvement on a method for preparing a hydrophobic film on the surface of a material. The method is characterized in that: irregular micro-nano protuberant structures are generated by bombarding a basis material by using a high-energy iron beam; a transition layer is formed by using ion implanting technology; and the hydrophobic film is formed by performing chemical vapor deposition or reactive magnetic sputtering. The method for preparing the hydrophobic film on the surface of the material comprises the following steps of: washing the surface of the basis material; bombarding the surface of the basis material to generate the micro-nano protuberant structures by using the high-energy iron beam; forming the transition layer by using the iron implanting technology; and forming the hydrophobic film by performing the chemical vapor deposition or the reactive magnetic sputtering. The surface of the film of the invention has bionic-like morphology and super-hydrophobic performance; the formed micro-nano structures are easier to clean; roots are not easy to break; and the hydrophobic film which is grown on the roots has the advantages of high bonding force, not easy drop, long service life and the like.
Description
Technical field
The invention belongs to substrate material surface modification technology field, relate to improvement substrate material surface hydrophobic film preparation method.
Background technology
Wetting property is meant the wetting behavior of liquid at solid surface, and solid surface is a critical nature of material surface to the wettability of liquid, is determined jointly by the chemical property and the microtexture of material surface.The wetting property of material can be weighed by the contact angle of liquid and solid surface, for liquid water, usually will be called water-wetted surface less than 90 ° solid surface with water contact angle, be called hydrophobic surface greater than 90 °, be called super hydrophobic surface with water contact angle greater than 150 ° surface, be called ultra-hydrophilic surface less than 15 ° surface with the contact angle of water.In the actual production practice, utilize surface engineering technology can change the material surface performance, make it have unique hydrophobic property, thereby can be with a wide range of applications in national defence, daily life and numerous industrial or agricultural field, as printing and dyeing and waterproof, material of construction waterproof, high-tension cable and electric porcelain insulator waterproof and ice, the naval vessels drag reduction of fabric, aircraft is moistureproof and anti-icing, the anti-ice and snow of solar cell etc., also can be applicable to the shell of windshield glass, water-heater and the medicine equipment etc. of automobile and aircraft etc.In natural organic evolution process, many animals and plants surface has demonstrated super-hydrophobicity.Super-hydrophobic and self-cleaning character as lotus leaf is known very early, and water droplet is in almost balling-up shape of lotus leaf surface and be easy to tumble.Barthlott and Neinhuis think that by the microtexture of observing the lotus leaf surface this self-cleaning feature is to be caused jointly by the micro-meter scale mastoid process of uneven surface and the existence of surperficial wax.The wax crystallization has hydrophobicity, so when water and this class surface contacts, can form the globule because of surface tension, adds the helping of fine structure of leaf table, and the globule of rolling can be taken away the particle of some dust mud in passing together, reaches the effect of oneself's cleaning.Utilize surface engineering technology to improve the material surface hydrophobic performance at present both at home and abroad, mainly form the micro-nano raised structures of hydrophobic surface by chemical method.For example, " Preparation of transparent superhydrophobic boehmite and silica films by sublimation of aluminum acetylacetonate ", Young kwon Kang etc., Adv.Mater., 1999,11:1365-1368.In the literary composition, Watanabe group utilizes chemical method to obtain the film that porous has the nano level roughness, modifies silicon fluoride at film surface then, obtains surface and the based superhydrophobic thin films of water contact angle greater than 150 °.Though the hydrophobic film that above-mentioned employing chemical method preparation contains micro nano structure is simple to operation, the film bonding force of preparation is poor, and is easily aging, not shock-resistant.In addition, adopt lithographic method and carbon nano tube growth method to form the micro nano structure of ordered array formula in addition." Reversible swithing superhydrophilicity and superhydrophobicity " T.L.Sun etc., Angew.Chem.Int.Ed., 2004,43:357-360.In the literary composition, employing laser ablation technology such as Sun form many grooves at silicon chip surface, utilize then the surface cause the atom transfer radical polymerization technology from the teeth outwards grafting form a strata sec.-propyl propylene phthalein amine " molecular brush ", thereby obtain having super-hydrophobic-super hydrophilic reversible " switch " surface of temperature response: when envrionment temperature is higher than 40 ℃, contact angle shows superhydrophobic property greater than 150 °; Envrionment temperature is lower than 25 ℃, and contact angle is Superhydrophilic matter near 0 °.Adopt etching method to carry out surface micronano structure processing,, pollute easily because structural arrangement is neatly tight, not easy to clean, simultaneously, though the film bonding force of this array structure preparation is better than chemical method,, also rupture from root easily, come off from matrix, and, complex process, cost height.
Summary of the invention
The objective of the invention is: propose a kind of low-cost preparation method of based superhydrophobic thin films with bionical shape micro-nano structure, high adhesive force and characteristics such as easy to clean.
Technical scheme of the present invention is: a kind of method for preparing hydrophobic film on material surface, it is characterized in that, utilize high energy ion beam that body material is bombarded to produce random micro-nano raised structures, and utilize ion implantation technique to form transition layer, carry out chemical vapour deposition or reaction magnetocontrol sputtering at last and form hydrophobic film, the step of preparation is as follows:
1, clean substrate material surface:
1.1, body material is carried out ultrasonic cleaning: body material is put into the container that deionized water is housed, carry out ultrasonic cleaning, scavenging period is 20~40 minutes, takes out then to dry up;
1.2, substrate material surface carried out acetone clean: be stained with acetone to piece surface wiping three times with clean gauze, dry up then;
1.3, use the ECR gas ion source of ion implantation and depositing device that piece surface is carried out ion sputtering to clean: body material is put on the Stage microscope of vacuum chamber, is vacuumized, when air pressure is lower than 4 * 10
-3During Pa, feed argon gas, make air pressure remain on 5 * 10 to vacuum chamber
-2Pa~8 * 10
-2Pa opens gas ion source, the negative bias that matrix applies more than the 500V is cleaned, till matrix surface does not have spark phenomenon;
2, make substrate material surface produce the micro-nano raised structures by the high energy ion beam bombardment:
Regulating argon flow amount, to make the air pressure of vacuum chamber be 0.06Pa~0.08Pa, opens high-voltage power supply, and regulating the high-voltage power supply frequency is 500Hz~800Hz, and pulse width is 2 μ s~10 μ s, voltage amplitude is-and 40kV~-60kV, bombardment time is 40min~60min;
3, ion implantation formation transition layer: close high-voltage power supply, it is 0.06Pa~0.08Pa that the adjusting argon flow amount makes the air pressure of vacuum chamber, the distance of regulating between sputtering target and the Stage microscope is 100mm~130mm, regulating the sputtering target electric current is 1A~2A, opens high-voltage power supply, and regulating the high-voltage power supply frequency is 500Hz~800Hz, pulse width is 2 μ s~5 μ s, voltage amplitude is-15kV~-30kV, carry out the transition layer preparation, injection length is controlled to be 20min~60min;
4, hydrophobic film deposition: deposit hydrophobic film according to one of following method:
4.1, fluorine carbon hydrophobic film: close high-voltage power supply, close argon gas, feed fluoro-gas, it is 0.06Pa~0.1Pa that the adjustments of gas flow makes the air pressure of vacuum chamber, opens the action of low-voltage pulse grid bias power supply, and the adjusting supply frequency is 40kHz~60kHz, dutycycle is 25%~50%, bias voltage is-100V~-200V, carry out fluorine carbon hydrophobic film deposition, depositing time is 50min~80min;
4.2, metal oxide film, be one of following substances: TiO
2, Al
2O
3: close high-voltage power supply, it is 0.06Pa~0.08Pa that the adjusting argon flow amount makes the air pressure of vacuum chamber, to make the air pressure of vacuum chamber be 0.08Pa~0.12Pa to aerating oxygen then, regulating the sputtering target electric current is 1A~2A, opens low pressure bias pulse power supply, and the adjusting supply frequency is 40kHz~60kHz, dutycycle is 25%~50%, bias voltage is-100V~-200V, carry out metal oxide hydrophobic film deposition, depositing time is 50min~80min.
Advantage of the present invention is: adopt the film of this method preparation to have bionical shape pattern and ultra-hydrophobicity, and the easier cleaning of the micro-nano structure of formation, root is difficult for rupturing; Have advantages such as bonding force height, difficult drop-off and long service life.This method is the hydrophobic film preparation method that a kind of technology is simple, low-cost, be suitable for industrial application.
Embodiment
Below the present invention is described in further details.A kind of method that on material surface, prepares hydrophobic film, it is characterized in that, utilize high energy ion beam that body material is bombarded to produce random micro-nano raised structures, and utilize ion implantation technique to form transition layer, carry out chemical vapour deposition or reaction magnetocontrol sputtering at last and form the hydrophobic film preparation, the step of preparation is as follows:
1, clean substrate material surface:
1.1, body material is carried out ultrasonic cleaning: body material is put into the container that deionized water is housed, carry out ultrasonic cleaning, scavenging period is 20~40 minutes, takes out then to dry up;
1.2, substrate material surface carried out acetone clean: be stained with acetone to piece surface wiping three times with clean gauze, dry up then;
1.3, use the ECR gas ion source of ion implantation and depositing device that piece surface is carried out ion sputtering to clean: body material is put on the Stage microscope of vacuum chamber, is vacuumized, when air pressure is lower than 4 * 10
-3During Pa, feed argon gas, make air pressure remain on 5 * 10 to vacuum chamber
-2Pa~8 * 10
-2Pa opens gas ion source, the negative bias that matrix applies more than the 500V is cleaned, till matrix surface does not have spark phenomenon;
2, make substrate material surface produce the micro-nano raised structures by the high energy ion beam bombardment:
Regulating argon flow amount, to make the air pressure of vacuum chamber be 0.06Pa~0.08Pa, opens high-voltage power supply, and regulating the high-voltage power supply frequency is 500Hz~800Hz, and pulse width is 2 μ s~10 μ s, voltage amplitude is-and 40kV~-60kV, bombardment time is 40min~60min;
3, ion implantation formation transition layer: close high-voltage power supply, it is 0.06Pa~0.08Pa that the adjusting argon flow amount makes the air pressure of vacuum chamber, the distance of regulating between sputtering target and the Stage microscope is 100mm~130mm, regulating the sputtering target electric current is 1A~2A, opens high-voltage power supply, and regulating the high-voltage power supply frequency is 500Hz~800Hz, pulse width is 2 μ s~5 μ s, voltage amplitude is-15kV~-30kV, carry out the transition layer preparation, injection length is controlled to be 20min~60min;
4, hydrophobic film deposition: deposit hydrophobic film according to one of following method:
4.1, fluorine carbon hydrophobic film: close high-voltage power supply, close argon gas, feed fluoro-gas, it is 0.06Pa~0.1Pa that the adjustments of gas flow makes the air pressure of vacuum chamber, opens the action of low-voltage pulse grid bias power supply, and the adjusting supply frequency is 40kHz~60kHz, dutycycle is 25%~50%, bias voltage is-100V~-200V, carry out fluorine carbon hydrophobic film deposition, depositing time is 50min~80min;
4.2, metal oxide film, be one of following substances: TiO
2, Al
2O
3: close high-voltage power supply, it is 0.06Pa~0.08Pa that the adjusting argon flow amount makes the air pressure of vacuum chamber, to make the air pressure of vacuum chamber be 0.08Pa~0.12Pa to aerating oxygen then, regulating the sputtering target electric current is 1A~2A, opens low pressure bias pulse power supply, and the adjusting supply frequency is 40kHz~60kHz, dutycycle is 25%~50%, bias voltage is-100V~-200V, carry out metal oxide hydrophobic film deposition, depositing time is 50min~80min.
Principle of work of the present invention is:
The hydrophobic performance of material can be weighed by the contact angle of liquid and solid surface by its surface energy and the common decision of surface microstructure.The present invention adopts high energy ion beam to bombard compound low energy ion beam depositing operation to prepare hydrophobic film, at first utilize high energy ion beam that body material is bombarded to produce random micro-nano raised structures, this raised structures is because height is in picturesque disorder and root is thicker, so easier cleaning, more firm with matrix bond, the generation of micro-nano raised structures can increase the roughness of material surface, improve the contact angle of material surface and water, and then utilize ion implantation technique between matrix and hydrophobic film, to form transition layer, to increase the sticking power between film and matrix, carry out chemical vapour deposition or reaction magnetocontrol sputtering at last again and prepare hydrophobic film (as fluorine carbon film, thin film of titanium oxide etc.), to reduce the surface energy of material surface, further improve the hydrophobic performance of material.
Embodiment 1: the fluorine carbon hydrophobic film preparation of micro-nano raised structures
1, clean substrate material surface:
1.1, body material is carried out ultrasonic cleaning: body material is put into the container that deionized water is housed, carry out ultrasonic cleaning, scavenging period is 40 minutes, takes out then to dry up;
1.2, substrate material surface carried out acetone clean: be stained with acetone to piece surface wiping three times with clean gauze, dry up then;
1.3, use the ECR gas ion source of ion implantation and depositing device that piece surface is carried out ion sputtering to clean: body material is put on the Stage microscope of vacuum chamber, is vacuumized, when air pressure is lower than 4 * 10
-3During Pa, feed argon gas, make air pressure remain on 6 * 10 to vacuum chamber
-2Pa opens gas ion source, the negative bias that matrix applies more than the 500V is cleaned, till matrix surface does not have spark phenomenon;
2, make substrate material surface produce the micro-nano raised structures by the high energy ion beam bombardment:
It is 8 * 10 that the adjusting argon flow amount makes the air pressure of vacuum chamber
-2Pa opens high-voltage power supply, and regulating the high-voltage power supply frequency is 800Hz, and pulse width is 2 μ s, and voltage amplitude is-50kV that bombardment time is 45min;
3, carbon ion injects and forms transition layer: close high-voltage power supply, it is 6 * 10 that the adjusting argon flow amount makes the air pressure of vacuum chamber
-2Pa, the distance of regulating between C sputtering target and the Stage microscope is 115mm, regulating C sputtering target electric current is 2A, open high-voltage power supply, regulating the high-voltage power supply frequency is 800Hz, and pulse width is 2 μ s, voltage amplitude is-20kV, carries out the preparation of C transition layer, and injection length is controlled to be 40min;
4, fluorine carbon hydrophobic film deposition:
Close high-voltage power supply, close argon gas, feed CF
4It is 7 * 10 that gas, adjustments of gas flow make the air pressure of vacuum chamber
-2Pa opens the action of low-voltage pulse grid bias power supply, and adjustings supply frequency is 50kHz, and dutycycle is 30%, and bias voltage is-150V, carries out fluorine carbon hydrophobic film and deposits, and depositing time is 60min.
Embodiment 2: the fluorine carbon hydrophobic film preparation of micro-nano raised structures
1, clean substrate material surface:
1.1, body material is carried out ultrasonic cleaning: body material is put into the container that deionized water is housed, carry out ultrasonic cleaning, scavenging period is 40 minutes, takes out then to dry up;
1.2, substrate material surface carried out acetone clean: be stained with acetone to piece surface wiping three times with clean gauze, dry up then;
1.3, use the ECR gas ion source of ion implantation and depositing device that piece surface is carried out ion sputtering to clean: body material is put on the Stage microscope of vacuum chamber, is vacuumized, when air pressure is lower than 4 * 10
-3During Pa, feed argon gas, make air pressure remain on 8 * 10 to vacuum chamber
-2Pa opens gas ion source, the negative bias that matrix applies more than the 500V is cleaned, till matrix surface does not have spark phenomenon;
2, make substrate material surface produce the micro-nano raised structures by the high energy ion beam bombardment:
It is 6 * 10 that the adjusting argon flow amount makes the air pressure of vacuum chamber
-2Pa opens high-voltage power supply, and regulating the high-voltage power supply frequency is 500Hz, and pulse width is 5 μ s, and voltage amplitude is-60kV that bombardment time is 60min;
3, carbon ion injects and forms transition layer: close high-voltage power supply, it is 6 * 10 that the adjusting argon flow amount makes the air pressure of vacuum chamber
-2Pa, the distance of regulating between C sputtering target and the Stage microscope is 120mm, regulating C sputtering target electric current is 1.5A, open high-voltage power supply, regulating the high-voltage power supply frequency is 500Hz, and pulse width is 5 μ s, voltage amplitude is-20kV, carries out the transition layer preparation, and injection length is controlled to be 40min;
4, fluorine carbon hydrophobic film deposition:
Close high-voltage power supply, close argon gas, feed C
3F
8It is 0.1Pa that gas, adjustments of gas flow make the air pressure of vacuum chamber, opens the action of low-voltage pulse grid bias power supply, and adjustings supply frequency is 40kHz, and dutycycle is 30%, and bias voltage is-180V, carries out fluorine carbon hydrophobic film and deposits, and depositing time is 80min.
Embodiment 3: the titanium oxide hydrophobic film preparation of micro-nano raised structures
1, clean substrate material surface:
1.1, body material is carried out ultrasonic cleaning: body material is put into the container that deionized water is housed, carry out ultrasonic cleaning, scavenging period is 40 minutes, takes out then to dry up;
1.2, substrate material surface carried out acetone clean: be stained with acetone to piece surface wiping three times with clean gauze, dry up then;
1.3, use the ECR gas ion source of ion implantation and depositing device that piece surface is carried out ion sputtering to clean: body material is put on the Stage microscope of vacuum chamber, is vacuumized, when air pressure is lower than 4 * 10
-3During Pa, feed argon gas, make air pressure remain on 8 * 10 to vacuum chamber
-2Pa opens gas ion source, the negative bias that matrix applies more than the 500V is cleaned, till matrix surface does not have spark phenomenon;
2, make substrate material surface produce the micro-nano raised structures by the high energy ion beam bombardment:
It is 6 * 10 that the adjusting argon flow amount makes the air pressure of vacuum chamber
-2Pa opens high-voltage power supply, and regulating the high-voltage power supply frequency is 800Hz, and pulse width is 5 μ s, and voltage amplitude is-60kV that bombardment time is 60min;
3, Ti injects and forms transition layer: close high-voltage power supply, it is 6 * 10 that the adjusting argon flow amount makes the air pressure of vacuum chamber
-2Pa, the distance of regulating between Ti sputtering target and the Stage microscope is 120mm, regulating Ti sputtering target electric current is 1.5A, open high-voltage power supply, regulating the high-voltage power supply frequency is 500Hz, and pulse width is 2 μ s, voltage amplitude is-20kV, carries out the transition layer preparation, and injection length is controlled to be 20min;
4, titanium dioxide hydrophobic film deposition:
Close high-voltage power supply, aerating oxygen, it is 1.2 * 10 that adjusting argon gas and oxygen gas flow make the air pressure of vacuum chamber
-1Pa regulates the sputtering target electric current to 1.5A, opens the action of low-voltage pulse grid bias power supply, and adjustings supply frequency is 50kHz, and dutycycle is 30%, and bias voltage is-150V, carries out the oxide compound hydrophobic film and prepares, and depositing time is 60min.
Claims (1)
1. method that on material surface, prepares hydrophobic film, it is characterized in that, utilize high energy ion beam that body material is bombarded to produce random micro-nano raised structures, and utilize ion implantation technique to form transition layer, carry out chemical vapour deposition or reaction magnetocontrol sputtering at last and form hydrophobic film, the step of preparation is as follows:
1.1, clean substrate material surface:
1.1.1, body material is carried out ultrasonic cleaning: body material is put into the container that deionized water is housed, carry out ultrasonic cleaning, scavenging period is 20~40 minutes, takes out then to dry up;
1.1.2, substrate material surface carried out acetone clean: be stained with acetone to piece surface wiping three times with clean gauze, dry up then;
1.1.3, use the ECR gas ion source of ion implantation and depositing device that piece surface is carried out ion sputtering to clean: body material is put on the Stage microscope of vacuum chamber, is vacuumized, when air pressure is lower than 4 * 10
-3During Pa, feed argon gas, make air pressure remain on 5 * 10 to vacuum chamber
-2Pa~8 * 10
-2Pa opens gas ion source, the negative bias that matrix applies more than the 500V is cleaned, till matrix surface does not have spark phenomenon;
1.2, make substrate material surface produce the micro-nano raised structures by high energy ion beam bombardment:
Regulating argon flow amount, to make the air pressure of vacuum chamber be 0.06Pa~0.08Pa, opens high-voltage power supply, and regulating the high-voltage power supply frequency is 500Hz~800Hz, and pulse width is 2 μ s~10 μ s, voltage amplitude is-and 40kV~-60kV, bombardment time is 40min~60min;
1.3, ion implantation formation transition layer: close high-voltage power supply, it is 0.06Pa~0.08Pa that the adjusting argon flow amount makes the air pressure of vacuum chamber, the distance of regulating between sputtering target and the Stage microscope is 100mm~130mm, regulating the sputtering target electric current is 1A~2A, opens high-voltage power supply, and regulating the high-voltage power supply frequency is 500Hz~800Hz, pulse width is 2 μ s~5 μ s, voltage amplitude is-15kV~-30kV, carry out the transition layer preparation, injection length is controlled to be 20min~65min;
1.4, hydrophobic film deposition: according to one of following method deposition hydrophobic film:
1.4.1, fluorine carbon hydrophobic film: close high-voltage power supply, close argon gas, feed fluoro-gas, it is 0.06Pa~0.1Pa that the adjustments of gas flow makes the air pressure of vacuum chamber, opens the action of low-voltage pulse grid bias power supply, and the adjusting supply frequency is 40kHz~60kHz, dutycycle is 25%~50%, bias voltage is-100V~-200V, carry out fluorine carbon hydrophobic film deposition, depositing time is 50min~80min;
1.4.2, metal oxide film, be one of following substances: TiO
2, Al
2O
3: close high-voltage power supply, it is 0.06Pa~0.08Pa that the adjusting argon flow amount makes the air pressure of vacuum chamber, to make the air pressure of vacuum chamber be 0.08Pa~0.12Pa to aerating oxygen then, regulating the sputtering target electric current is 1A~2A, opens low pressure bias pulse power supply, and the adjusting supply frequency is 40kHz~60kHz, dutycycle is 25%~50%, bias voltage is-100V~-200V, carry out metal oxide hydrophobic film deposition, depositing time is 50min~80min.
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