CN105483614B - A kind of diamond-like micro-pipe and preparation method thereof - Google Patents

A kind of diamond-like micro-pipe and preparation method thereof Download PDF

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CN105483614B
CN105483614B CN201510874097.3A CN201510874097A CN105483614B CN 105483614 B CN105483614 B CN 105483614B CN 201510874097 A CN201510874097 A CN 201510874097A CN 105483614 B CN105483614 B CN 105483614B
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diamond
micro
pipe
substrate
preparation
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CN105483614A (en
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汪爱英
焦圆
柯培玲
张栋
郭鹏
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0005—Separation of the coating from the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5873—Removal of material

Abstract

The present invention relates to three-dimensional structure field of material technology, and in particular to a kind of preparation method of diamond-like micro-pipe comprising following steps: (1) providing a substrate, and carries out surface etching treatment to the substrate；(2) the surface deposited metal doped diamond carbon film for using magnetron sputtering and substrate of the linear ion beam co-electrodeposition method after etching, wherein the metal includes at least one of copper, aluminium, silver；(3) the substrate for being deposited with metal-doped diamond-like carbon film is placed in acid solution and is soaked for a period of time, so that the metal in the metal-doped diamond-like carbon film is dissolved, diamond-like carbon film crimps under the action of compression, obtains the diamond-like micro-pipe with hollow structure.The present invention also provides a kind of diamond-like micro-pipes.Preparation method of the invention is simple, is suitble to industrialization, the diameter and thickness of obtained diamond-like micro-pipe is micron order, and can be regulated and controled by the operating current and sedimentation time of controlled sputtering source, with good application prospect.

Description

A kind of diamond-like micro-pipe and preparation method thereof
Technical field
The present invention relates to three-dimensional structure field of material technology more particularly to a kind of diamond-like micro-pipe and preparation method thereof.
Background technique
In fields such as treatment of cancer, organizational engineering, basal cell researchs, using micrometer structure or nanostructure to biology Cell is adjusted and control has very important significance.It is at present that growing environment has obtained extensively with microarray, microflute etc. General research.However, microarray, microflute etc. are only capable of providing the environment of two-dimensional structure to regulate and control to cell growth.But due to Biological cell is to the sensibility of environment, and often there are larger differences in two-dimensional environment in organism three-dimensional environment for biological cell It is different.Existing research report, a kind of hereditary information expression of the nerve cell in three-dimensional substrates and the hereditary information in two-dimentional substrate It is different.Therefore, synthesis three-dimensional structure is particularly important to carry out cell adjusting.In various three-dimensional structures, micron tube structure is similar Biological body vessel can preferably simulate the growth behavior of cell in vivo.However, since cell volume is smaller, and It is difficult to prepare and the comparable micro-tubular structure of cell volume.
Diamond-like carbon film has the characteristics that good cell compatibility, blood compatibility and elasticity, chemical inertness, is one The very promising biomaterial of kind.
Summary of the invention
In view of this, diamond-like micro-pipe and its preparation side it is necessory to provide a kind of adjustable micro-pipe diameter and thickness Method.
The present invention provides a kind of preparation method of diamond-like micro-pipe comprising following steps:
(1) a substrate is provided, and surface etching treatment is carried out to the substrate；
(2) class is adulterated using magnetron sputtering and the surface deposited metal of substrate of the linear ion beam co-electrodeposition method after etching Diamond-like carbon film；
(3) the substrate for being deposited with metal-doped diamond-like carbon film is placed in acid solution and is soaked for a period of time, so that institute The metal stated in metal-doped diamond-like carbon film is dissolved, and diamond-like carbon film crimps under the action of compression, The diamond-like micro-pipe with hollow structure is obtained, wherein the metal includes at least one of copper, aluminium, silver.
Further, carrying out surface etching treatment to the substrate in step (1) is specially that substrate is placed in vacuum cavity In, linear ion source is opened, the first inert gas is passed through, while applying the pulsed negative bias of 50V~300V to the substrate, and Realize the etching to the substrate, wherein the operating current of linear ion source is 0.1A~0.5A, first inert gas Being passed through flow is 20sccm~50sccm, and etch period is 2 minutes~10 minutes.
Further, step (2) described in magnetron sputtering and linear ion beam co-electrodeposition method specially open simultaneously linearly from Component and controlled sputtering source, controlled sputtering source are metallic target, are passed through hydrocarbon gas to linear ion source, are passed through to controlled sputtering source Second inert gas, at the same to the substrate apply 100V~300V pulsed negative bias.
Further, step (2) described in hydrocarbon gas be acetylene or methane, the flow that is passed through of the hydrocarbon gas is 15sccm~50sccm.
Further, step (2) described in the second inert gas be argon gas, the flow that is passed through of second inert gas is 15sccm~80sccm.
Further, step (2) described in linear ion source operating current be 0.1A~0.5A, the work of linear ion source The rate of doing work is 100W~1000W, and the operating current of the controlled sputtering source is 1A~5A, and the operating power of controlled sputtering source is 300W~3000W.
Further, in step, (2) the middle time deposited is 5 minutes~180 minutes.
Further, step (2) described in metal-doped diamond-like carbon film the atomic percent of metal be 1%~40%.
Further, the acid solution is concentrated sulfuric acid solution, concentrated nitric acid solution or hydrochloric acid solution, and the time of the immersion is 2 minutes~60 minutes.
The present invention also provides a kind of diamond-like micro-pipe obtained using above-mentioned preparation method, the diamond-like micro-pipe is One tubular structure with hollow space, the diameter of the diamond-like micro-pipe are 0.5 micron~20 microns, the diamond-like Micro-pipe with a thickness of 0.1 micron~5 microns.
Compared with prior art, diamond-like micro-pipe provided by the invention and preparation method thereof has the advantage that One, first by the way that the compression of diamond-like carbon film during the deposition process can be reduced, so to diamond-like carbon film doping metals Afterwards after with acid leach solution metal, the original deposition position of metallic atom will become hole, to disperse diamond-like The compression of stone carbon film, the surface of diamond-like carbon film will not crack at this time, but can occur under the action of compression Curling, forms the diamond-like micro-pipe of tubular；Second, it can be by the operating current of adjusting controlled sputtering source, to regulate and control metal original Son and then influences the size of compression in the doping of diamond-like carbon film, final to realize to the diameter of diamond-like micro-pipe It adjusts；Third can finally be realized micro- to diamond-like by adjusting the time of deposition to regulate and control the thickness of diamond-like carbon film The adjusting of the thickness of pipe.Preparation method is simple for this, easily operated, is suitble to industrialization.The obtained diamond-like micro-pipe Diameter and thickness be micron order, and can be regulated and controled by the operating current and sedimentation time of controlled sputtering source, the eka-gold Hard rock micro-pipe is with good application prospect.
Detailed description of the invention
Fig. 1 is the stereoscan photograph for the diamond-like micro-pipe that embodiment 1 obtains.
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned attached drawing.
Specific embodiment
Diamond-like micro-pipe provided by the invention and preparation method thereof will be described further below.
The present invention provides a kind of preparation method of diamond-like micro-pipe comprising following steps:
S1 provides a substrate, and carries out surface etching treatment to the substrate；
S2 adulterates class using magnetron sputtering and the surface deposited metal of substrate of the linear ion beam co-electrodeposition method after etching Diamond-like carbon film；And
The substrate for being deposited with metal-doped diamond-like carbon film is placed in acid solution and is soaked for a period of time by S3, so that Metal in the metal-doped diamond-like carbon film is dissolved, and diamond-like carbon film is rolled up under the action of compression Song obtains the diamond-like micro-pipe with hollow structure.
In step sl, by carrying out surface etching treatment to substrate, so that the surface cleaning of the substrate.The substrate Material can be for silicon, polyethylene terephthalate (abbreviation PET), polypropylene (abbreviation PP), glass etc..
Carrying out surface etching treatment to the substrate is specially that substrate is placed in vacuum cavity, opens linear ion source, It is passed through the first inert gas, while applying 50V~300V (pulsed negative bias, and realizing to the substrate to the substrate Etching.Wherein, the operating current of linear ion source is 0.1A~0.5A.The flow that is passed through of first inert gas is 20standard-state cubic centimeter per minute (abbreviation sccm)~50sccm.Etch period is 2 points Clock~10 minute.First inert gas can be argon gas.
In step s 2, gold while may be implemented in carbon atom deposition by magnetron sputtering and linear ion beam co-electrodeposition method Belong to atom also to deposit, to obtain metal-doped diamond-like carbon film.It, can be with by diamond-like carbon film doping metals atom Reduce the compression of diamond-like carbon film during the deposition process.The metallic atom is copper, aluminium, silver, this is because above-mentioned metal Carbide Phases cannot be formed with carbon atom, still with metallic forms Dispersed precipitate in diamond-like carbon film.
The magnetron sputtering and linear ion beam co-electrodeposition method specially open linear ion source and controlled sputtering source simultaneously, Controlled sputtering source is metal copper target, is passed through hydrocarbon gas to linear ion source, is passed through the second inert gas to controlled sputtering source, together When to the substrate apply 100V~300V pulsed negative bias.The hydrocarbon gas is acetylene or methane, the hydrocarbon gas Be passed through flow be 15sccm~50sccm.Second inert gas is argon gas.Second inert gas is passed through flow For 15sccm~80sccm.Second inert gas can be argon gas.Preferably, second inert gas and the first indifferent gas Body is identical.
The operating current of the linear ion source is 0.1A~0.5A, and operating power is 100W~1000W.Preferably, institute The operating current for stating linear ion source is 0.1A~0.3A, and operating power is 100W~500W.
The operating current of the controlled sputtering source is 1A~5A, and operating power is 300W~3000W.Preferably, the magnetic The operating current for controlling sputtering source is 2A~3A, and operating power is 600W~1500W, so that the doping of metal maintains preferably In range, and then make the diameter of the diamond-like micro-pipe in 10 microns.
The time of the deposition is 5 minutes~180 minutes.Preferably, the time of the deposition is 20 minutes~60 minutes.
The atomic percent of metal is 1%~40% in the metal-doped diamond-like carbon film.Preferably, the metal The atomic percent of metal is 10%~30% in doped diamond carbon film.
In step s3, it is impregnated by the way that the substrate for being deposited with metal-doped diamond-like carbon film to be placed in acid solution, Acid in acid solution reacts with metal and makes dissolving metal, and the original deposition position of metallic atom will become hole, from And having dispersed the compression of diamond-like carbon film, the surface of diamond-like carbon film will not crack, but can crimp, shape At the diamond-like micro-pipe of tubular.It is appreciated that dissolving metal is referred to gold under the action of acid solution by the acid solution Belong to atom whole or almost all is dissolved, and the hardly kish atom in diamond-like carbon film.It needs herein Illustrate, which is the tubular structure crimped by diamond-like carbon film, the side wall of the tubular structure It is not closed completely and continuous side wall for one, but there are one that the subtle seam formed is connected by the both ends of diamond-like carbon film Gap, this has no effect on the three-dimensional structure and related application of the diamond-like micro-pipe.
The acid solution can be concentrated sulfuric acid solution, concentrated nitric acid solution or hydrochloric acid solution.The concentration of the acid solution is not Limit, as long as metallic atom can be dissolved.When the acid solution is concentrated nitric acid solution or concentrated sulfuric acid solution, the acidity The mass fraction of solution is 65%~80%, preferably 65%~78%.The time of the immersion is 2 minutes~60 minutes.It is excellent Choosing, the time of the immersion is 5 minutes~30 minutes.
The present invention also provides a kind of diamond-like micro-pipes.The diamond-like micro-pipe is a tubular knot with hollow space Structure.The diameter of the diamond-like micro-pipe be 0.5 micron~20 microns, the diamond-like micro-pipe with a thickness of 0.1 micron~5 Micron.Preferably, the diameter of the diamond-like micro-pipe be 0.5 micron~10 microns, the diamond-like micro-pipe with a thickness of 0.3 micron~3 microns.
It should be noted that the diameter of the diamond-like micro-pipe refers to the outer diameter of the tubular structure, the diamond-like The thickness of micro-pipe refers to the outer diameter of tubular structure and the difference of internal diameter.
Diamond-like micro-pipe provided by the invention and preparation method thereof has the advantage that first, first by eka-gold Hard rock carbon film doping metals can reduce the compression of diamond-like carbon film during the deposition process, then molten with acid solution After solving metal, the original deposition position of metallic atom will become hole, thus dispersed the compression of diamond-like carbon film, this When diamond-like carbon film surface will not crack, but can be crimped under the action of compression, form the class of tubular Diamond micro-pipe；Second, it can be by the operating current of adjusting controlled sputtering source, to regulate and control metallic atom in diamond-like carbon film Doping, and then the size of compression is influenced, the final adjusting realized to the diameter of diamond-like micro-pipe；Third can pass through tune The time of deposition is saved, to regulate and control the thickness of diamond-like carbon film, the final adjusting realized to the thickness of diamond-like micro-pipe.This system Preparation Method is simple and easy, easily operated, is suitble to industrialization.The diameter and thickness of the obtained diamond-like micro-pipe is micron Grade, and can be regulated and controled by the operating current and sedimentation time of controlled sputtering source, which has preferable Application prospect.
Hereinafter, will further illustrate in conjunction with specific embodiments.
Embodiment 1
Surface etching treatment is carried out to silicon base first, it is specific: silicon base being put into and starts to vacuumize in cavity, true Reciprocal of duty cycle reaches 2.0 × 10-5When Pa, argon gas is passed through into cavity, the flow of argon gas is 35sccm, while applying 100V to silicon base Pulsed negative bias, open linear ion source, the operating current of linear ion source is 0.2A, using argon plasma to substrate Surface performs etching, etch period 10min.
Then class is adulterated using magnetron sputtering and the copper-depositing on surface of substrate of the linear ion beam co-electrodeposition method after etching Diamond-like carbon film, specific: after etching, the flow for adjusting argon gas is 65sccm, and being continually fed into flow is 15sccm's Acetylene gas opens controlled sputtering source and linear ion electron gun, and wherein the operating current of controlled sputtering source is 2A, linear ion source Operating current be 0.2A, while the basad back bias voltage for applying 100V, the frequency of negative bias pulsed power are 350KHz, pulse Width is 1.75 μ s, and the time of deposition is 40min.
Finally, it is 65.0wt%~68.0wt% that the substrate for being deposited with Copper-cladding Aluminum Bar diamond-like carbon film, which is placed in mass fraction, Concentrated nitric acid solution in impregnate 30min, obtain diamond-like micro-pipe.
The micro-pipe pattern of the obtained diamond-like micro-pipe please refers to Fig. 1.As seen from Figure 1, which has Hollow structure, the diameter of the diamond-like micro-pipe are about 2 microns, and thickness is about 0.7 micron.
Embodiment 2
Surface etching treatment is carried out to silicon base first, it is specific: silicon base being put into and starts to vacuumize in cavity, true Reciprocal of duty cycle reaches 2.0 × 10-5When Pa, argon gas is passed through into cavity, the flow of argon gas is 35sccm, while applying 100V to silicon base Pulsed negative bias, open linear ion source, the operating current of linear ion source is 0.2A, using argon plasma to substrate Surface performs etching, etch period 10min.
Then class is adulterated using the surface deposition of aluminum of magnetron sputtering and substrate of the linear ion beam co-electrodeposition method after etching Diamond-like carbon film, specific: after etching, the flow for adjusting argon gas is 65sccm, and being continually fed into flow is 15sccm's Acetylene gas opens controlled sputtering source and linear ion electron gun, and wherein the operating current of controlled sputtering source is 3A, linear ion source Operating current be 0.2A, while the basad back bias voltage for applying 100V, the frequency of negative bias pulsed power are 350KHz, pulse Width is 1.75 μ s, and the time of deposition is 60min.
Finally, it is 20.0wt%~35.0wt% that the substrate for being deposited with aluminium doped diamond carbon film, which is placed in mass fraction, Hydrochloric acid solution in impregnate 30min, obtain diamond-like micro-pipe.
Embodiment 3
Surface etching treatment is carried out to silicon base first, it is specific: silicon base being put into and starts to vacuumize in cavity, true Reciprocal of duty cycle reaches 2.0 × 10-5When Pa, argon gas is passed through into cavity, the flow of argon gas is 35sccm, while applying 100V to silicon base Pulsed negative bias, open linear ion source, the operating current of linear ion source is 0.2A, using argon plasma to substrate Surface performs etching, etch period 10min.
Then Ag doping class is deposited using the surface of magnetron sputtering and substrate of the linear ion beam co-electrodeposition method after etching Diamond-like carbon film, specific: after etching, the flow for adjusting argon gas is 65sccm, and being continually fed into flow is 15sccm's Acetylene gas opens controlled sputtering source and linear ion electron gun, and wherein the operating current of controlled sputtering source is 2A, linear ion source Operating current be 0.3A, while the basad back bias voltage for applying 100V, the frequency of negative bias pulsed power are 350KHz, pulse Width is 1.75 μ s, and the time of deposition is 20min.
Finally, it is 65.0wt%~68.0wt% that the substrate for being deposited with Ag doping diamond-like carbon film, which is placed in mass fraction, Concentrated nitric acid solution in impregnate 30min, obtain diamond-like micro-pipe.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest scope of cause.

Claims (10)

1. a kind of preparation method of diamond-like micro-pipe comprising following steps:
(1) a substrate is provided, and surface etching treatment is carried out to the substrate；
(2) diamond-like is adulterated using magnetron sputtering and the surface deposited metal of substrate of the linear ion beam co-electrodeposition method after etching Stone carbon film, wherein the metal includes at least one of copper, aluminium, silver；
(3) the substrate for being deposited with metal-doped diamond-like carbon film is placed in acid solution and is soaked for a period of time, so that the gold The metal belonged in doped diamond carbon film is dissolved, and diamond-like carbon film crimps under the action of compression, obtains Diamond-like micro-pipe with hollow structure.
2. the preparation method of diamond-like micro-pipe as described in claim 1, which is characterized in that in step (1) to the substrate Carrying out surface etching treatment is specially that substrate is placed in vacuum cavity, opens linear ion source, is passed through the first inert gas, together When apply the pulsed negative bias of 50V~300V to the substrate, and realize to the etching of the substrate, wherein linear ion source Operating current be 0.1A~0.5A, first inert gas be passed through flow be 20sccm~50sccm, etch period 2 Minute~10 minutes.
3. the preparation method of diamond-like micro-pipe as described in claim 1, which is characterized in that step (2) described in magnetic control splash It penetrates and linear ion beam co-electrodeposition method specifically: while linear ion source and controlled sputtering source are opened, controlled sputtering source is metal Target is passed through hydrocarbon gas to linear ion source, is passed through the second inert gas to controlled sputtering source, while applying to the substrate The pulsed negative bias of 100V~300V.
4. the preparation method of diamond-like micro-pipe as claimed in claim 3, which is characterized in that step (2) described in carburetted hydrogen gas Body is acetylene or methane, and the flow that is passed through of the hydrocarbon gas is 15sccm~50sccm.
5. the preparation method of diamond-like micro-pipe as claimed in claim 3, which is characterized in that step (2) described in it is second lazy Property gas be argon gas, second inert gas be passed through flow be 15sccm~80sccm.
6. the preparation method of diamond-like micro-pipe as claimed in claim 3, which is characterized in that step (2) described in linearly from The operating current of component is 0.1A~0.5A, and the operating power of linear ion source is 100W~1000W, the controlled sputtering source Operating current is 1A~5A, and the operating power of controlled sputtering source is 300W~3000W.
7. the preparation method of diamond-like micro-pipe as described in claim 1, which is characterized in that step (2) in deposit time It is 5 minutes~180 minutes.
8. the preparation method of diamond-like micro-pipe as described in claim 1, which is characterized in that step (2) described in it is metal-doped The atomic percent of metal is 1%~40% in diamond-like carbon film.
9. the preparation method of diamond-like micro-pipe as described in claim 1, which is characterized in that step (3) described in acid solution For concentrated sulfuric acid solution, concentrated nitric acid solution or hydrochloric acid solution, the time of the immersion is 2 minutes~60 minutes.
10. a kind of diamond-like micro-pipe obtained using the preparation method as described in any one of claim 1~9, which is characterized in that The diamond-like micro-pipe is a tubular structure with hollow space, the diameter of the diamond-like micro-pipe is 0.5 micron~ 20 microns, the diamond-like micro-pipe with a thickness of 0.1 micron~5 microns.
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CN102472963A (en) * 2009-07-03 2012-05-23 Hoya株式会社 Function-gradient inorganic resist, substrate with function-gradient inorganic resist, cylindrical substrate with function-gradient inorganic resist, method for forming function-gradient inorganic resist, method for forming fine pattern, and inorgani
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