CN105779965B - A method of porous doped diamond film is prepared using particle beams control technique - Google Patents
A method of porous doped diamond film is prepared using particle beams control technique Download PDFInfo
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- CN105779965B CN105779965B CN201610037867.3A CN201610037867A CN105779965B CN 105779965 B CN105779965 B CN 105779965B CN 201610037867 A CN201610037867 A CN 201610037867A CN 105779965 B CN105779965 B CN 105779965B
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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
A method of porous diamond-like (DLC) film being adulterated using the preparation of particle beams control technique, belongs to field of inorganic nano material.The invention utilizes magnetic filtering cathode arc precipitation equipment, using nickel source as cathode, using carbonaceous gas as precursor gas, in certain particle beams Parameter Conditions sinking carbon distribution base nickel nano compound film, its structure is that nickel metallic particles is dispersed in the amorphous carbon phase of surrounding, and only a small amount of nickle atom is entrained in amorphous carbon phase.The thin-film material chemical solution prepared is corroded, removes the nickel metal phase in film and the nickle atom that retains amorphous carbon phase and wherein adulterate, can be obtained after being rinsed with deionized water and adulterate porous DLC film.By controlling the particle beams parameter in experiment, i.e. realization pore diameter, void density, SP3 key relative amount and the regulatable porous DLC film material of doping of doping in film.This method is easy to operate, and short preparation period simultaneously can realize the mass production for adulterating porous DLC film material.
Description
Technical field
The present invention relates to field of inorganic nano-material preparation, more particularly to one kind to prepare porous doping by particle beams regulation
The method of diamond-like (DLC) film.
Background technique
Porous carbon materials refer to the carbon material with different pore structures, due to highly developed pore structure, greatly
Specific surface area, the features such as higher chemical stability, high mechanical stability and electric conductivity, in adsorption of metal ions, catalyst
The fields such as carrier, hydrogen storage, supercapacitor and fuel cell show huge application potential.And the porous carbon materials adulterated can
With the electron transfer rate for greatly changing the surface texture of material, changing its cellular structure, improving material, to expand more
Hole carbon material is more widely applied in every field.The method for preparing porous doping carbon material at present mainly has activation method and mould
Plate method.Using the often unordered porous carbon materials of carbonization-activation method preparation, it is difficult to control its hole road shape and aperture；It utilizes
Template, which can prepare to provide, will have high surface area, structurally ordered, pore volume larger and the uniform porous carbon of pore size distribution
Material, but preparation process is cumbersome, the period is longer, and template uses so that preparation cost greatly improves, and is difficult to realize industry
Using.Diamond-like (Diamond-like carbon, DLC) film belongs to one of carbon material, contains diamond lattic structure
(SP3Hybrid bond) and graphite-structure (SP2Hybrid bond), carbon atom is mainly with SP3And SP2Hybrid bond combines.The film is by moral at first
State scholar Aisenberg has amorphous carbon similar with diamond feature using the preparation of carbon ion beam enhanced deposition technology
Film, and it is defined as DLC.DLC film has many excellent properties similar with diamond thin, is being permitted as new function material
It is multi-field to have huge application prospect, but do not have the report for preparing porous doping DLC film at present.
Summary of the invention
Hole is prepared by ion beam regulation using magnetic filtering cathode arc precipitation equipment (FCVAD) the invention discloses a kind of
The method of size and the regulatable porous DLC film material of doping of doping.
The technical scheme adopted by the invention is that: magnetic filtering cathode arc precipitation equipment is utilized, the nickel for being 99.99% with purity
For cathode, being passed through carbonaceous gas is that precursor gas passes through the nickel of electric arc starter cathode under certain Parameter Conditions and vacuum degree
Source generates self-holding arc discharge in cathode surface, evaporates the nickel material of cathode, obtain the plasma of nickel.The nickel of generation
Violent collision occurs for the gas in plasma and chamber, is adequately ionized the gas in chamber, generates hybrid plasma.
These plasmas are in the bend pipe by being wound by copper coil, big in plasma due to the magneticaction inside bend pipe
Particle and some neutral particles are filtered, and the remaining particle beams is deposited under the action of negative substrate bias with certain energy
On silicon substrate, to prepare fine and close and smooth surface Ni/DLC nano compound film.Due to nickel and the lower parent of carbon
And property, the knot of the nano composite structure that the film prepared separates for DLC phase with nickel metal phase, as amorphous carbon package nickel crystallite
Structure, only extremely a small amount of nickle atom are blended in the amorphous carbon phase of surrounding.Wherein in film nickel crystallite size and film
Middle SP3The relative amount of key can include the throughput for being passed through gas, back bias voltage and deflection magnetic by adjusting the parameter of the particle beams
Field current changes, and the thickness of film can obtain by different sedimentation times.The nano compound film of preparation is placed in 3M
Hydrochloric acid solution or 70wt% nitric acid solution in corrode, can remove the nickel metal phase in film, and amorphous carbon phase and its
In the nickle atom that adulterates on a small quantity do not influenced by solution then, it is regulatable to form pore diameter, film thickness and doping
Porous doping DLC film material.
Ni/DLC nano compound film preparation method: it is nano combined thin that Ni/DLC is deposited on the silicon substrate of clean surface
Film, which is that the plasma that metal nickel source generates nickel is triggered by cathode arc, in nickel plasma and chamber
Carbonaceous gas collide and make gas ionization, the hybrid plasma after ionization pass through magnetic filter when it is big therein
Grain and neutral particle are filtered, and the remaining particle beams is deposited on silicon substrate under the action of back bias voltage with certain energy,
Form crystallite dimension, thickness and SP3The regulatable phase of key relative amount separates Ni/DLC nano compound film.
It is further preferred that applying the back bias voltage of 100~1000V by 90% duty ratio on a silicon substrate.
It is further preferred that metal arc source is nickel source, the arc stream that triggering nickel source forms nickel plasma is 80~120A, will
The electric current that pdp filter removes the wherein bend pipe magnetic field of bulky grain and neutral particle is 1.0~2.0A, the back bias voltage of extraction
For 100~1000V.
It is further preferred that the DLC phase in Ni/DLC film be carbon containing precursor gas by being passed through by nickel ion collide from
Change forms carbon -containing plasma, and back bias voltage is filtered and drawn by magnetic filter and is deposited on substrate to be formed with certain energy
's.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 deposition time be 0.1h~1h, obtained nano compound film with a thickness of 0.5um~
5um。
The preparation method of porous doping DLC film: the Ni/DLC nano compound film of preparation is corroded using chemical method
Obtain porous doping DLC film.
It is further preferred that the solution of chemical attack is concentrated nitric acid or hydrochloric acid solution, concentration when corrosion is 70wt.%
Concentrated nitric acid, 3M hydrochloric acid.
It is further preferred that the time of corrosion is 30s~for 24 hours.
Beneficial outcomes of the invention are that the magnetic filtering cathode arc precipitation equipment that the present invention uses can effectively filter out greatly
Particle and neutral particle, the remaining particle beams are deposited on substrate i.e. under the extraction effect of certain back bias voltage with certain energy
The nano compound film that smooth densification can be obtained is made by simply regulating and controlling the test parameters of magnetic filtering cathode arc precipitation equipment
The line and energy of the equal particles beams change and obstructed thickness, crystallite dimension and SP can be obtained3The carbon nickel phase of key relative amount
Isolated nano compound film.By the nickel metal phase in chemical solution erosion removal nickel/DLC laminated film, nickel can be obtained
Doping, film thickness and pore diameter and SP3The regulatable porous DLC film structure of doping of key relative amount, preparation
Method is convenient and efficient.And this porous DLC for regulating and controlling preparation different aperture diameter, thickness and doping by ion beam is thin
The method of membrane material, which can be also used for mutually separating nanocomposite by carbon-iron, carbon-cobalt, carbon-copper, prepares porous LDC film
Material.
Detailed description of the invention
It is illustrated by attached drawing and specific embodiment, features described above of the invention and advantage will become more clear
It Chu and is readily appreciated that.
Fig. 1 is magnetic filtering cathode arc precipitation equipment schematic diagram.
Drawing reference numeral explanation:
101- silicon substrate, 102- nickel cathode source, 103- acetylene/methane air inlet, 104- nitrogen inlet, 105- negative bias
Pressure, 106- magnetic filter, 107- Magnetic filter coil, 108- observation window, 109- pump interface.
Fig. 2 is the crystallite dimension of nano compound film with the typical change tendency chart of gas flow.
Fig. 3 is the C1s map of the XPS of nano compound film.
Fig. 4 is the SP of nano compound film3Key relative amount with gas flow and back bias voltage typical change tendency chart.
Fig. 5 is the SEM figure of the sample in cross section of Ni/DLC nano compound film corrosion front and back.
Fig. 6 is the SEM figure of the sample in cross section of Ni/CNx nano compound film corrosion front and back.
Fig. 7 is the EDS figure of the sample in cross section of Ni/DLC nano compound film corrosion front and back.
Fig. 8 is the EDS figure of the sample in cross section of Ni/CNx nano compound film corrosion front and back.
Fig. 9 is component content pair in Ni/DLC nano compound film and Ni/CNx nano compound film corrosion front and back film
Than.
Specific embodiment
It is described with reference to the drawings, the detailed present invention that introduces is using the doping of regulation particle beams parameter preparation different aperture size
Two kinds of implementation methods of porous DLC film, but the present invention is not limited to provided embodiment.
Embodiment one:
1. raw material:
(1) nickel source that purity is 99.99%, methane gas, 2cm*2cm silicon wafer.
(2) alcoholic solution, acetone soln.
(3) hydrochloric acid 50ml, deionized water 50ml.
2. preparation method:
(1) silicon substrate cleans: being cleaned by ultrasonic using alcohol and acetone soln to silicon wafer.
(2) preparation of Ni/DLC nano compound film: depositing (FCVAD) device using magnetic filtering cathode arc, is yin with nickel
Pole adjusts the parameter of magnetic filtering cathode arc precipitation equipment are as follows: vacuum 3*10- using methane as precursor gas3Pa, arc stream 100A,
Negative pressure 200V, magnetic deflection field electric current 2A, methane gas flow are 20sccm.Under this Parameter Conditions, with the 2cm*2cm's that cleaned
Silicon wafer is substrate, and sedimentation time 20min prepares the Ni/DLC nano compound film that thickness is about 1um.
(3) preparation of the porous DLC film of nickel is adulterated: at room temperature, by the salt of Ni/DLC nano compound film submergence 3M
In acid solution about for 24 hours, according to formula 2Ni+6HCl → 2NiCl3+3H2Metallic nickel is all dissolved by chemical reaction.It will corrosion
Sample afterwards takes out, and is cleaned by ultrasonic with deionized water, is finally placed in baking oven and dries in 70 DEG C of environment.
Embodiment two:
1. raw material:
(1) nickel source that purity is 99.99%, acetylene gas, nitrogen, 2cm*2cm silicon wafer.
(2) alcoholic solution, acetone soln.
(3) nitric acid 50ml, deionized water 50ml.
2. preparation method:
(1) silicon substrate cleans: being cleaned by ultrasonic using alcohol and acetone soln to silicon wafer.
(2) preparation of Ni/CNx nano compound film: depositing (FCVAD) device using magnetic filtering cathode arc, is yin with nickel
Pole adjusts the parameter of magnetic filtering cathode arc precipitation equipment are as follows: vacuum 3* using the mixed gas of acetylene and nitrogen as precursor gas
10-3Pa, arc stream 100A, negative pressure 200V, magnetic deflection field electric current 2A, acetylene throughput are 40sccm, and stream of nitrogen gas amount is 20sccm.
Under this Parameter Conditions, using the silicon wafer of the 2cm*2cm cleaned as substrate, sedimentation time 20min makes under this Parameter Conditions
Standby Ni/CNx nano compound film.
(3) preparation of the porous doping DLC film of rich nitrogen: at room temperature, Ni/CNx nano compound film is immersed in
In the nitric acid solution of 70wt%, according to formula Ni+4HNO3→Ni(NO3)2+2NO2+2H2O is molten by metallic nickel by chemically reacting
Solution.Sample after corrosion is taken out, is cleaned by ultrasonic with deionized water, is finally placed in baking oven and is dried in 70 DEG C of environment.
Fig. 2 is trend chart of the typical film crystallite dimension with the throughput being passed through.As can be seen from Figure, with
The crystallite dimension of the change nano compound film of throughput is also changed, and illustrating can be to film by changing test parameters
In metal grain size generate Effective Regulation, and then change corrosion after porous DLC film pore-size and density.Fig. 3 is
The C1s map of typical nano compound film photoelectron spectroscopy (XPS) carries out swarming fitting by the spectral line to C1S, can obtain
The SP into film2And SP3The relative amount of key.Fig. 4 is SP in film3The relative amount of key with throughput and back bias voltage variation,
As can be seen from Figure, the change of throughput and negative pressure is to SP in film3The relative amount of key produces apparent influence, and thin
SP in film3Relative amount and hardness, the coefficient of friction of film of key etc. have a close influence, thus can by regulation back bias voltage and
Gas flow controls SP in film3The relative amount of key, and then influence the performance of porous DLC film after corrosion.Fig. 5 is Ni/
The Cross Section Morphology of DLC nano compound film corrosion front and back sample.By comparison as can be seen that corrosion rear film is apparent porous
Structure, and pore diameter is 10nm or so, it is almost the same with the crystallite dimension in Fig. 2.Fig. 6 is respectively Ni/CNx nano combined thin
The Cross Section Morphology of sample before and after erosion.By comparison as can be seen that the pattern of film is the structure of spherical accumulation before corrosion,
And the porous structure of apparent Nano grade is then formed after corroding.Fig. 7 and Fig. 8 is respectively Ni/DLC nano compound film and Ni/
The essential element content balance figure of CNx nano compound film corrosion front and back sample.It can be found that the nickel in corrosion first two film
Atom accounts for leading, and the peak intensity of nickle atom obviously weakens after corrosion and carbon, nitrogen peak are occupied an leading position.Ni/DLC in Fig. 9
The relative amount of element is than being more clear in nano compound film and Ni/CNx nano compound film corrosion front and back film sample
It illustrates by corroding the metallic element that can be effectively removed in film: about by nickle atom content after can be seen that corrosion in table
For 2at%, illustrate that the nickel in film sample is substantially all and be corroded, only a small amount of nickel is entrained in porous DLC film.It is right
In sample after the corrosion of Ni/CNx nano compound film, N/C atomic ratio is about 0.33, illustrates the rich nitrogen prepared by this method
The nitrogen content of porous doping DLC film is relatively high, thus has and be more widely applied effect.
Compared with prior art, each implementation of the invention has the advantage that
(1) preparation method is easy to operate, short preparation period.
(2) preparation cost is lower, and can realize prepared by batch.
(3) pore diameter of the porous DLC film of doping prepared by is in Nano grade.
(4) throughput, the back bias voltage, deflection being such as passed through by adjusting the particle beams parameter of magnetic filtering cathode arc precipitation equipment
Field supply is, it can be achieved that pore diameter, film thickness and SP3The control of key relative amount.
(5) selection for not needing additionally to heat therefore substrate during preparing film is more extensive, such as silicon, glass, no
Become rusty steel, polyester material.
(6) metal phase in the nano compound film that this method is mentioned is nickel metal, but this method is not limited to nickel,
The preparation of porous doping DLC material can be achieved in copper, iron, cobalt, the gold separated with carbon phase.
It should be noted that the above content is combine specific embodiment made for the present invention further specifically
It is bright, and it cannot be said that a specific embodiment of the invention is only limitted to this, under above-mentioned introduction of the invention, those skilled in the art can
To carry out various improvement and deformations on the basis of the above embodiments, and these are improved or deformation falls in protection model of the invention
In enclosing.It will be understood by those skilled in the art that specific descriptions above are intended merely to explain the purpose of the present invention, it is not intended to limit
The system present invention.Protection scope of the present invention is defined by the claims and their equivalents.
Claims (7)
1. a kind of method for preparing porous doping DLC film using particle beams control technique, it is characterised in that the following steps are included:
Step 1, using magnetic filtering cathode arc precipitation equipment using nickel as cathode arc source, using carbonaceous gas as precursor gas, certain
Parameter Conditions and vacuum degree under, using monocrystalline silicon as substrate preparation comprising face-centred cubic metal nickel crystallite Ni/DLC nanometer answer
Close film；
Step 2 corrodes Ni/DLC nano compound film with hydrochloric acid or nitric acid solution, the control corrosion rate time, obtains described more
Adulterate DLC film in hole.
2. the method according to claim 1 for preparing porous doping DLC film using particle beams control technique, feature exist
In: the nano compound film prepared in step 1 is phase separation structure, i.e., doping is wrapped up around the nickel metal phase of face-centred cubic structure
The amorphous carbon phase of a small amount of nickle atom.
3. the method according to claim 1 for preparing porous doping DLC film using particle beams control technique, feature exist
In: substrate used can be changed to stainless steel, steel alloy, high-speed steel, glass, polyester material when preparing nano compound film in step 1
Material.
4. the method according to claim 1 for preparing porous doping DLC film using particle beams control technique, feature exist
In: by adjusting the beam energy parameter of magnetic filtering cathode arc precipitation equipment including being passed through gas flow, negative bias in step 1
Pressure, magnetic deflection field electric current are, it can be achieved that porous pore diameter, density and the SP for adulterating DLC film3The regulation of relative amount.
5. the method according to claim 1 for preparing porous doping DLC film using particle beams control technique, feature exist
In: pass through chemical equation 2Ni+6HCl → 2NiCl in step 23+3H2And Ni+4HNO3→Ni(NO3)2+2NO2+2H2O will be thin
Nickel metal phase in film erodes, and retains the amorphous carbon phase of doping nickle atom.
6. the method according to claim 1 for preparing porous doping DLC film using particle beams control technique, feature exist
In: by changing the throughput of acetylene and nitrogen ratio in magnetic filtering cathode arc precipitation equipment, it can be achieved that the porous doping DLC of rich nitrogen is thin
The regulation of carbon-nitrogen ratio in film.
7. the method according to claim 1 for preparing porous doping DLC film using particle beams control technique, feature exist
In: the etch is applied equally to prepare porous doping DLC using carbon-copper, carbon-cobalt, carbon-metallographic separation nano compound film
Thin-film material.
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| CN109518159B (en) * | 2018-11-21 | 2020-12-04 | 中国科学院大学 | Method for growing diamond by codoping transition metal elements and nitrogen |
| CN110055506B (en) * | 2019-06-12 | 2021-08-31 | 中国科学院宁波材料技术与工程研究所 | Preparation method of metal-doped porous carbon film |
| 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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| CN103613094A (en) * | 2013-11-28 | 2014-03-05 | 华中科技大学 | Method for preparing graphene and porous amorphous carbon films simultaneously |
| CN103643217A (en) * | 2013-11-28 | 2014-03-19 | 华中科技大学 | Method for preparing self-supporting graphite porous amorphous carbon thin film |
| CN103681900A (en) * | 2013-12-25 | 2014-03-26 | 厦门大学 | Ni-doped crystalline silicon intermediate zone material and preparation method thereof |
| CN104178745A (en) * | 2013-05-28 | 2014-12-03 | 中国科学院金属研究所 | Method for manufacturing porous diamond or porous cubic silicon carbide self-supporting film |
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| TWI372111B (en) * | 2007-12-28 | 2012-09-11 | Ind Tech Res Inst | Structural material of diamond like carbon complex films and method of manufacturing the same |
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| CN104178745A (en) * | 2013-05-28 | 2014-12-03 | 中国科学院金属研究所 | Method for manufacturing porous diamond or porous cubic silicon carbide self-supporting film |
| CN103613094A (en) * | 2013-11-28 | 2014-03-05 | 华中科技大学 | Method for preparing graphene and porous amorphous carbon films simultaneously |
| CN103643217A (en) * | 2013-11-28 | 2014-03-19 | 华中科技大学 | Method for preparing self-supporting graphite porous amorphous carbon thin film |
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