CN105779965A - Method for preparing porous doped diamond-like carbon thin film by utilizing particle beam control technology - Google Patents
Method for preparing porous doped diamond-like carbon thin film by utilizing particle beam control technology Download PDFInfo
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- CN105779965A CN105779965A CN201610037867.3A CN201610037867A CN105779965A CN 105779965 A CN105779965 A CN 105779965A CN 201610037867 A CN201610037867 A CN 201610037867A CN 105779965 A CN105779965 A CN 105779965A
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/278—Diamond only doping or introduction of a secondary phase in the diamond
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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Abstract
The invention provides a method for preparing a doped porous diamond-like carbon (DLC) thin film by utilizing the particle beam control technology and belongs to the field of inorganic nano materials. According to the method for preparing the doped porous DLC thin film by utilizing the particle beam control technology, a magnetic filtered cathodic arc deposition device is utilized, a nickel source serves as a cathode, carbon-containing gas serves as the precursor gas, and a carbon-based nickel nano composite thin film is deposited under the condition of certain particle beam parameters and is of the structure that nickel metal particles are dispersed in surrounding amorphous carbon phases and only a small number of nickel atoms are doped in the amorphous carbon phases; the prepared thin film material is corroded through a chemical solution, nickel metal in the thin film is removed, the amorphous carbon phases and the nickel atoms doped in the amorphous carbon phases are retained, and the doped porous DLC thin film can be obtained after the thin film is washed with deionized water; and by controlling the particle beam parameters in the experiment, the doped porous DLC thin film material adjustable in pore diameter, pore density and SP3 key relative content and doping amount in the thin film is achieved. The method for preparing the doped porous DLC thin film by utilizing the particle beam control technology is easy to operate, short in preparation period and capable of achieving mass production of the doped porous DLC thin film material.
Description
Technical field
The present invention relates to field of inorganic nano-material preparation, particularly relate to a kind of method by particle beam regulation and control preparation porous doped diamond (DLC) thin film.
Background technology
Porous carbon materials refers to the material with carbon element with different pore structures, owing to having highly developed pore structure, big specific surface area, the features such as higher chemical stability, high mechanical stability and electric conductivity, demonstrate huge application potential in fields such as adsorption of metal ions, catalyst carrier, hydrogen storage, ultracapacitor and fuel cells.And the porous carbon materials adulterated can greatly change the surface texture of material, change its pore passage structure, improves the electron transfer rate of material, is more widely applied thus expanding porous carbon materials in every field.The method preparing porous doping carbon material at present mainly has activation method and template.Utilize unordered porous carbon materials often prepared by carbonization-activation method, be difficult to control its duct shape and aperture；Utilize template to prepare to provide and high surface, structurally ordered, pore volume will be had relatively big and the uniform porous carbon materials of pore size distribution, but preparation process is loaded down with trivial details, the cycle is longer, and the use of template makes preparation cost be greatly improved, and is difficulty with commercial Application.Diamond like carbon (Diamond-likecarbon, DLC) thin film belongs to the one in material with carbon element, and containing diamond lattic structure (SP3 hybrid bond) and graphite-structure (SP2 hybrid bond), carbon atom mainly combines with SP3 and SP2 hybrid bond.This film is utilized prepared by carbon ion beam enhanced deposition technology to have and the amorphous carbon film of diamond feature similarity by German scholar Aisenberg at first, and is defined as DLC.DLC film has many excellent properties similar to diamond thin, has huge application prospect as new function material in a lot of fields, but does not have the report of preparation porous doping DLC film at present.
Summary of the invention
The invention discloses one utilizes magnetic filtering cathode arc precipitation equipment (FCVAD) to be prepared pore size and the method for doping all regulatable doping porous DLC film material by ion beam regulation and control.
The technical solution adopted in the present invention is: utilize magnetic filtering cathode arc precipitation equipment, with purity be 99.99% nickel for negative electrode, passing into carbonaceous gas is precursor gas, under certain Parameter Conditions and vacuum, nickel source by electric arc starter cathode, produce the arc discharge controlled oneself at cathode surface, make the nickel material of negative electrode evaporate, obtain the plasma of nickel.There is violent collision with the gas in chamber in the nickel plasma produced, makes the gas in chamber be adequately ionized, and produces hybrid plasma.These plasmas are when the bend pipe by being wound around by copper coil, magneticaction within bend pipe, bulky grain in plasma and some neutral particles are filtered, remaining particle beam under the effect of negative substrate bias with on certain energy deposition to silicon substrate, thus preparing densification and the smooth Ni/DLC nano compound film of surfacing.Due to nickel and the relatively low affinity of carbon, the thin film prepared is the nano composite structure that DLC phase is separated with nickel metal, is the structure of amorphous carbon parcel nickel crystallite, only have extremely a small amount of nickle atom be blended in the amorphous carbon of surrounding mutually in.Wherein in thin film nickel crystallite size and in thin film the relative amount of SP3 key can include passing into the throughput of gas, back bias voltage and magnetic deflection field electric current etc. and change by adjusting the parameter of particle beam, the thickness of thin film can be obtained by different sedimentation times.The nano compound film of preparation is placed in the hydrochloric acid solution of 3M or the salpeter solution of 70wt% and corrodes, the nickel metal phase in thin film can be removed, the nickle atom of amorphous carbon phase and wherein a small amount of doping, then not by the impact of solution, forms all regulatable porous doping DLC film material of pore diameter, film thickness and doping.
Ni/DLC nano compound film prepares scheme: deposit Ni/DLC nano compound film on the silicon substrate of clean surface, this nano compound film is to trigger metal nickel source by cathode arc to produce the plasma of nickel, nickel plasma collides with the carbonaceous gas in chamber and makes gas ionization, hybrid plasma after ionization is filtered through magnetic filter bulky grain therein and neutral particle, remaining particle beam under the effect of back bias voltage with on certain energy deposition to silicon substrate, form crystallite dimension, thickness and all regulatable Ni/DLC nano compound film that is separated of SP3 key relative amount.
It is further preferred that apply the back bias voltage of 100～1000V on a silicon substrate by the dutycycle of 90%.
It is further preferred that metal arc source is nickel source, the arc stream triggering nickel source formation nickel plasma is 80～120A, and the electric current that pdp filter is removed the bend pipe magnetic field of wherein bulky grain and neutral particle is 1.0～2.0A, and the back bias voltage of extraction is 100～1000V.
It is further preferred that the DLC phase in Ni/DLC film is the precursor gas by the carbon containing passed into is formed carbon-containing plasma by nickel ion impact ionization, filter and draw what back bias voltage was formed on substrate with certain energy deposition through magnetic filter.The arc stream of deposition is 80～120A, and the electric current in bend pipe magnetic field is 1.0～2.0A, and the back bias voltage of extraction is 100～1000V.
It is further preferred that the time of deposition is 0.1h～1h, the thickness of the nano compound film obtained is 0.5um～5um.
The preparation scheme of porous doping DLC film: the Ni/DLC nano compound film of preparation utilizes chemical method corrosion obtain porous doping DLC film.
It is further preferred that the solution of chemical attack is concentrated nitric acid or hydrochloric acid solution, concentration during corrosion is the hydrochloric acid of the concentrated nitric acid of 70wt.%, 3M.
It is further preferred that the time of corrosion is 30s～24h.
The beneficial outcomes of the present invention is, the magnetic filtering cathode arc precipitation equipment that the present invention uses can effectively filter out bulky grain and neutral particle, remaining particle beam under the extraction effect of certain back bias voltage so that certain energy deposition to substrate can obtain the nano compound film of smooth densification, by simply regulating and controlling the test parameters of magnetic filtering cathode arc precipitation equipment, make to wait the line of particle beam and energy to change and can obtain the nano compound film that the carbon nickel of obstructed thickness, crystallite dimension and SP3 key relative amount is separated.By the nickel metal phase in chemical solution erosion removal nickel/DLC laminated film, can obtaining nickel doping, film thickness and pore diameter and SP3 key relative amount all regulatable doping porous DLC film structure, preparation method is convenient and swift.And this method by the porous DLC film material of ion beam regulation and control preparation different aperture diameter, thickness and doping can be also used for by Nano-composite materials porous LDC thin-film materials that is separated such as carbon-ferrum, carbon-cobalt, carbon-copper.
Accompanying drawing explanation
Being illustrated by accompanying drawing and detailed description of the invention, the features described above of the present invention and advantage will become apparent with easy to understand.
Fig. 1 is magnetic filtering cathode arc precipitation equipment schematic diagram；
Drawing reference numeral illustrates:
101-silicon substrate, 102-nickel cathode source, 103-acetylene/methane air inlet, 104-nitrogen inlet, 105-back bias voltage, 106-magnetic filter, 107-Magnetic filter coil, 108-observation window, 109-pump interface.
Fig. 2 is the crystallite dimension typical change trendgram with gas flow of nano compound film；
Fig. 3 is the C1s collection of illustrative plates of the XPS of nano compound film；
Fig. 4 is the SP3 key relative amount typical change trendgram with gas flow and back bias voltage of nano compound film；
Fig. 5 is the SEM figure of the sample in cross section before and after the corrosion of Ni/DLC nano compound film；
Fig. 6 is the SEM figure of the sample in cross section before and after the corrosion of Ni/CNx nano compound film；
Fig. 7 is the EDS figure of the sample in cross section before and after the corrosion of Ni/DLC nano compound film；
Fig. 8 is the EDS figure of the sample in cross section before and after the corrosion of Ni/CNx nano compound film；
Fig. 9 is component content contrast in thin film before and after Ni/DLC nano compound film and the corrosion of Ni/CNx nano compound film.
Detailed description of the invention
Accompanying drawings, the detailed two kinds of implementations introducing the doping porous DLC film that the present invention utilizes regulation and control particle beam parameter to prepare different aperture size, but the present invention is not limited to the embodiment that provides.
Embodiment one:
1. raw material:
(1) purity is the nickel source of 99.99%, methane gas, 2cm*2cm silicon chip；
(2) alcoholic solution, acetone soln；
(3) hydrochloric acid 50ml, deionized water 50ml.
2. preparation method:
(1) silicon substrate cleans: use ethanol and acetone soln that silicon chip is carried out ultrasonic cleaning.
(2) preparation of Ni/DLC nano compound film: utilize magnetic filtering cathode arc deposition (FCVAD) device, with nickel for carbon source, with methane for precursor gas, by the parameter adjustment of magnetic filtering cathode arc precipitation equipment be: vacuum 3*10-3Pa, arc stream 100A, negative pressure 200V, magnetic deflection field electric current 2A, methane gas flow is 20sccm.Under this Parameter Conditions, with the silicon chip of cleaned 2cm*2cm for substrate, sedimentation time is 20min, prepares the Ni/DLC nano compound film that thickness is about 1um.
(3) preparation of the porous DLC film of doping nickel: under room temperature, by about 24h in the hydrochloric acid solution of Ni/DLC nano compound film submergence 3M, according to formula 2Ni+6HCl → 2NiCl3+3H2By chemical reaction, metallic nickel is all dissolved.Sample after corrosion is taken out, uses deionized water ultrasonic cleaning, be finally placed in baking oven in the environment of 70 DEG C and dry.
Embodiment two:
1. raw material:
(1) purity is the nickel source of 99.99%, acetylene gas, nitrogen, 2cm*2cm silicon chip；
(2) alcoholic solution, acetone soln；
(3) nitric acid 50ml, deionized water 50ml.
2. preparation method:
(1) silicon substrate cleans: use ethanol and acetone soln that silicon chip is carried out ultrasonic cleaning.
(2) preparation of Ni/CNx nano compound film: utilize magnetic filtering cathode arc deposition (FCVAD) device, with nickel for carbon source, with the mixing gas of acetylene and nitrogen for precursor gas, by the parameter adjustment of magnetic filtering cathode arc precipitation equipment it is: vacuum 3*10-3Pa, arc stream 100A, negative pressure 200V, magnetic deflection field electric current 2A, acetylene gas flow is 40sccm, and stream of nitrogen gas amount is 20sccm.Under this Parameter Conditions, with the silicon chip of cleaned 2cm*2cm for substrate, sedimentation time is 20min, prepares Ni/CNx nano compound film under this Parameter Conditions.
(3) preparation of rich nitrogen porous doping DLC film: under room temperature, Ni/CNx nano compound film is immersed in the salpeter solution of 70wt%, according to formula Ni+4HNO3→Ni(NO3)2+2NO2+2H2Metallic nickel is dissolved by O by chemical reaction.Sample after corrosion is taken out, uses deionized water ultrasonic cleaning, be finally placed in baking oven in the environment of 70 DEG C and dry.
Fig. 2 is the typical thin film crystallite dimension changing trend diagram with the throughput passed into.As can be seen from Figure, along with the crystallite dimension changing nano compound film of throughput also there occurs change, illustrate the metal grain size in thin film to produce Effective Regulation by changing test parameters, and then change the pore-size of porous DLC film and density after corrosion.Fig. 3 is the C1s collection of illustrative plates of typical nano compound film photoelectron spectroscopy (XPS), by the spectral line of C1S is carried out swarming matching, can obtain the relative amount of SP2 and SP3 key in thin film.Fig. 4 be in thin film the relative amount of SP3 key with the change of throughput and back bias voltage, as can be seen from Figure, the relative amount of SP3 key in thin film is created obvious impact by the change of throughput and negative pressure, and the relative amount of SP3 key and the hardness of thin film, coefficient of friction etc. have close impact in thin film, therefore the relative amount of SP3 key in thin film and then the performance of porous DLC film after impact corrosion can be controlled by regulation and control back bias voltage and gas flow.Fig. 5 is the Cross Section Morphology of sample before and after the corrosion of Ni/DLC nano compound film.By contrasting it can be seen that corroding rear film is obvious loose structure, and pore diameter is about 10nm, basically identical with the crystallite dimension in Fig. 2.The Cross Section Morphology of sample before and after the corrosion of Fig. 6 respectively Ni/CNx nano compound film.By contrasting it can be seen that the pattern of thin film is the structure of spherical accumulation before corrosion, after corrosion, then form the loose structure of obvious Nano grade.The essential element content balance figure of sample before and after Fig. 7 and Fig. 8 respectively Ni/DLC nano compound film and the corrosion of Ni/CNx nano compound film.It is found that the nickle atom in corrosion first two thin film all accounts for leading, after corrosion, the peak intensity of nickle atom substantially weakens and occupy an leading position in carbon, nitrogen peak.Ni/DLC nano compound film and Ni/CNx nano compound film in Fig. 9 corrode the relative amount of element in the film sample of front and back and describe by corroding the metallic element that can effectively remove in thin film than what become apparent from: be about 2at% by nickle atom content after can be seen that corrosion in table, illustrate that the nickel in film sample is substantially all to be corroded, only have a small amount of nickel and be entrained in porous DLC film.In sample after corroding for Ni/CNx nano compound film, N/C atomic ratio is about 0.33, illustrates that the adulterate nitrogen content of DLC film of the rich nitrogen porous prepared by the method is of a relatively high, thus has and be more widely applied effect.
Compared with prior art, each enforcement of the present invention has the advantage that
(1) this preparation method is simple to operate, and manufacturing cycle is short；
(2) preparation cost is relatively low, and can realize batch preparation；
(3) pore diameter of the doping porous DLC film prepared by is at Nano grade；
(4) by adjusting the particle beam parameter such as the throughput passed into, back bias voltage, magnetic deflection field electric current etc. of magnetic filtering cathode arc precipitation equipment, it may be achieved the control of pore diameter, film thickness and SP3 key relative amount；
(5) selection that need not additionally heat therefore substrate in the process of thin film is prepared more extensive, such as silicon, glass, rustless steel, polyester material etc.；
(6) metal in the nano compound film that the method is mentioned is mutually for nickel metal, but the method is not limited to nickel, and the copper that is separated with carbon, ferrum, cobalt, gold etc. all can realize porous and adulterate the preparation of DLC material；
It should be noted that; above content is in conjunction with specific embodiment further description made for the present invention; it cannot be assumed that the specific embodiment of the present invention is only limitted to this; under the above-mentioned instruction of the present invention; those skilled in the art can carry out various improvement and deformation on the basis of above-described embodiment, and these improve or deformation is within the scope of the present invention.It will be understood by those skilled in the art that specific descriptions above are intended merely to the explanation purpose of the present invention, be not intended to limit the present invention.Protection scope of the present invention is limited by claim and equivalent thereof.
Claims (7)
1. one kind utilizes the method that particle beam control technique prepares porous doping DLC film, it is characterised in that comprise the following steps:
Step 1, utilize magnetic filtering cathode arc precipitation equipment with nickel for cathode arc source, with carbonaceous gas for precursor gas, prepare Ni/DLC nano compound film with monocrystal silicon for substrate；
Step 2, corrode Ni/DLC nano compound film, control corrosion rate time with hydrochloric acid or salpeter solution, obtain described porous doping DLC film.
2. the method utilizing particle beam control technique to prepare porous doping DLC film according to claim 1, it is characterised in that: in step 1, the nano compound film of preparation is phase separation structure, and namely nickel metal around wraps up the amorphous carbon phase of a small amount of nickle atom that adulterates mutually.
3. the method utilizing particle beam control technique to prepare porous doping DLC film according to claim 1, it is characterised in that: substrate used when preparing nano compound film in step 1 can be changed to rustless steel, steel alloy, high-speed steel, glass, polyester material etc..
4. the method utilizing particle beam regulation and control preparation porous doping DLC film according to claim 1, it is characterized in that: step 1 includes passing into gas flow, back bias voltage, magnetic deflection field electric current etc. by the beam energy parameter of adjustment magnetic filtering cathode arc precipitation equipment, it may be achieved the regulation and control of the porous doping pore diameter of DLC film, density and SP3 relative amount.
5. the method utilizing particle beam control technique to prepare porous doping DLC film according to claim 1, it is characterised in that: by chemical equation 2Ni+6HCl → 2NiCl in step 23+3H2And Ni+4HNO3→Ni(NO3)2+2NO2+2H2Nickel metal in thin film is eroded by O mutually, and retains the amorphous carbon phase of doping nickle atom.
6. the method utilizing particle beam control technique to prepare porous doping DLC film according to claim 1, it is characterized in that: by changing the throughput ratio of acetylene and nitrogen in magnetic filtering cathode arc precipitation equipment, it may be achieved the regulation and control of the carbon-nitrogen ratio in rich nitrogen porous doping DLC film.
7. the method utilizing particle beam control technique preparation doping porous DLC film according to claim 1, it is characterised in that: this etch is applied equally to utilize the nano compound films that are separated such as carbon-copper, carbon-cobalt, carbon-Jin to prepare porous doping DLC film material.
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Cited By (3)
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| CN109518159A (en) * | 2018-11-21 | 2019-03-26 | 中国科学院大学 | A kind of method of transiting group metal elements and nitrogen co-doped growth diamond |
| CN110055506A (en) * | 2019-06-12 | 2019-07-26 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of metal-doped porous C film |
| CN110760815A (en) * | 2019-11-22 | 2020-02-07 | 惠州市三航无人机技术研究院 | Preparation method of porous doped diamond-like carbon film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109518159A (en) * | 2018-11-21 | 2019-03-26 | 中国科学院大学 | A kind of method of transiting group metal elements and nitrogen co-doped growth diamond |
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| CN110760815B (en) * | 2019-11-22 | 2021-11-19 | 惠州市三航无人机技术研究院 | Preparation method of porous doped diamond-like carbon film |
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