CN107164728B - A kind of preparation method of N ion dopings thin film of ceria - Google Patents

A kind of preparation method of N ion dopings thin film of ceria Download PDF

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CN107164728B
CN107164728B CN201710427185.8A CN201710427185A CN107164728B CN 107164728 B CN107164728 B CN 107164728B CN 201710427185 A CN201710427185 A CN 201710427185A CN 107164728 B CN107164728 B CN 107164728B
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magnetron sputtering
ceo
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CN107164728A (en
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安涛
邓晓芳
王爽
刘淑杰
高玉欣
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Changchun University
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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
    • C23C14/0641—Nitrides
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/5846—Reactive treatment
    • C23C14/5853—Oxidation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
    • H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
    • H01M8/126—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing cerium oxide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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Abstract

The present invention provides a kind of N3‑Adulterate CeO2The preparation method of film, in Ar and N2Mixed atmosphere in, using metal Ce as target, CeN films are obtained through magnetron sputtering, by CeN film oxidations obtained to get N3‑Adulterate CeO2Film.N has been made using magnetron sputtering simultaneously in the present invention under cryogenic3‑Adulterate CeO2Solid-oxide fuel battery electrolyte film, problem of environmental pollution caused by need to using high temperature and organic solvent using chemical preparation process in the past is overcome, and has many advantages, such as the good material homogeneity prepared, thickness controllable precise compared with traditional chemical routes, is firmly combined with substrate, nano-crystal film can be prepared.

Description

A kind of preparation method of N ion dopings thin film of ceria
Technical field
The present invention relates to solid-oxide fuel battery electrolyte technical field of film preparation more particularly to a kind of N ions Adulterate CeO2The preparation method of film.
Background technology
Solid oxide fuel cell (SOFC) is a kind of fuel gas and oxidant gas to be passed through ion-conductive oxide Occur electrochemistry in conjunction with and all solid state energy conversion device that produces electricl energy.Electrolyte in traditional SOFC is Y2O3Stable ZrO2(being abbreviated as YSZ), must could obtain ideal oxygen ionic conductivity under high temperature (900~1000 DEG C), and CeO2Base is electrolysed Oxygen ionic conductivity ratio YSZ of the matter under medium temperature (500~800 DEG C) is higher by several times, is ground in recent years to medium temperature electrolyte Study carefully work and all concentrates on the CeO with cubic fluorite structure mostly2On sill.
Pure CeO2Conductivity is relatively low, its conductivity can be improved by the method for doping.N3-Ion can also be used as one kind Doped source adjusts the performance of oxide.Generally use chemical method prepares N in the prior art3-Ion doping CeO2Sill. Jorge etc. (referring to《Nitrogen Doping of Ceria》,Chem.Mater.2008,20:1682-1684) ammonolysis is used The method of reaction in a reducing atmosphere, is prepared for N in 550~900 DEG C of temperature ranges3-Ion doping CeO2Sill, N3-From Sub- doping concentration has reached 4.5%；But there are problems that synthesis temperature is higher (550~900 DEG C).Mao etc. (referring to 《Synthesis,characterization and computational study of nitrogen-doped CeO2nanoparticles with visible-light activity》, Phys.Chem.Chem.Phys., 2008,10: 5633~5638) N is prepared for using wet-chemical route3-Ion doping CeO2Sill, N3-Ion doping is at concentrations up to 11%；But It is to use a large amount of organic solvent in the synthesis process, easily causes problem of environmental pollution.
Invention content
In view of this, the purpose of the present invention is to provide a kind of N ion dopings CeO2The preparation method of film, in low temperature item N ion dopings CeO is prepared under part2Solid-oxide fuel battery electrolyte film overcomes and uses chemical preparation process in the past Problem of environmental pollution caused by high temperature and organic solvent need to be used.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
A kind of N ion dopings CeO2The preparation method of film, includes the following steps：
(1) in Ar and N2Mixed atmosphere in, using metal Ce as target, CeN films are obtained through magnetron sputtering；
(2) by CeN film oxidations made from the step (1) to get N ion dopings CeO2Film.
Preferably, the sputtering pressure of magnetron sputtering is 0.8~2.0Pa in the step (1).
Preferably, the radio-frequency power of magnetron sputtering is 50~200W in the step (1).
Preferably, the time of magnetron sputtering is 2~4 hours in the step (1).
Preferably, the temperature of magnetron sputtering is 25~200 DEG C in the step (1).
Preferably, the gas flow of Ar is 30~60cm in the step (1)3/ min, the N2Gas flow be 5~ 10cm3/min。
Preferably, the substrate used when magnetron sputtering in the step (1) is single crystalline Si.
Preferably, oxidation carries out in air in the step (2).
Preferably, the time of the oxidation is 2~30 days.
Preferably, the temperature of the oxidation is 20~25 DEG C.
The present invention provides a kind of N ion dopings CeO2The preparation method of film, in Ar and N2Mixed atmosphere in, with gold Category Ce is target, CeN films is prepared through magnetron sputtering, by CeN film oxidations obtained to get N3-Adulterate CeO2Film. N has been made using magnetron sputtering simultaneously in the present invention under cryogenic3-Adulterate CeO2Solid-oxide fuel battery electrolyte is thin Film overcomes problem of environmental pollution caused by need to using high temperature and organic solvent using chemical preparation process in the past, and more traditional Chemical method have prepare material homogeneity is good, thickness controllable precise, with substrate is firmly combined with, can prepare nano-crystal film etc. Advantage, N obtained3-Adulterate CeO2N in film3-Ion maximum doping can reach 6.46%, N3-It is doped to CeO2Middle replacement Part O2-Ion can improve O2-Ionic vacancies concentration, and then improve N3-Adulterate CeO2Solid-oxide fuel battery electrolyte The ionic conductivity of film.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the XRD spectra of different oxidization time film samples in the embodiment of the present invention 1；
Fig. 2 is N in the embodiment of the present invention 13-Adulterate CeO2Film surface and N through Ar ion etchings after ten minutes3-Doping CeO2The XPS spectrum figure of film；
Fig. 3 is N in the embodiment of the present invention 13-Adulterate CeO2The scanning electron microscope (SEM) photograph of film, wherein 3 (a) is to be deposited on single crystalline Si N on substrate3-Adulterate CeO2The surface scan electron microscope of film, Fig. 3 (b) are the N being deposited on single crystal Si substrate3-Adulterate CeO2 The cross-sectional scans electron microscope of film.
Specific implementation mode
The present invention provides a kind of N ion dopings CeO2The preparation method of film, includes the following steps：
(1) in Ar and N2Mixed atmosphere in, using metal Ce as target, CeN films are obtained through magnetron sputtering；
(2) by CeN film oxidations made from the step (1) to get N3-Adulterate CeO2Film.
The present invention is in Ar and N2Mixed atmosphere in, using metal Ce as target, CeN films are obtained through magnetron sputtering.At this In invention, the gas flow of the Ar is preferably 30~60cm3/ min, more preferably 40~50cm3/min；The N2Gas Flow is preferably 5~10cm3/ min, more preferably 6~8cm3/min。
The present invention is preferably by the Ar and N2It is passed through in vacuum chamber or each leads into vacuum chamber simultaneously, the vacuum chamber Pressure is preferably 9.5 × 10-5~2.0 × 10-4Pa, more preferably 1.0 × 10-4~1.5 × 10-4Pa；The present invention is to magnetron sputtering Device there is no special restriction, using device well known to those skilled in the art.
The present invention does not have the substrate material used when the magnetron sputtering special restriction, using those skilled in the art Well known magnetron sputtering substrate；Substrate is preferably single crystalline Si in embodiments of the present invention.
In the present invention, the sputtering pressure of the magnetron sputtering is preferably 0.8~2.0Pa, more preferably 1~1.5Pa.
In the present invention, the radio-frequency power of the magnetron sputtering is preferably 50~200W, more preferably 100~150W.
In the present invention, the time of the magnetron sputtering is preferably 2~4 hours, more preferably 2.5~3.5 hours；It is described The temperature of magnetron sputtering is preferably 25~200 DEG C, more preferably 30~100 DEG C.
In the present invention, the thickness of the CeN films is preferably 100nm~600nm, more preferably 200nm~500nm.
After obtaining CeN films, the present invention is by CeN film oxidations to get N3-Adulterate CeO2Film.In the present invention, described The time of oxidation is preferably 2 days~30 days, more preferably 20 days~25 days；The temperature of the oxidation is preferably 20~25 DEG C, It is preferably carried out at room temperature in the embodiment of the present invention, does not need additional heating or cooling.
In the present invention, the N3-The thickness for adulterating CeN films is preferably 100nm~600nm, and more preferably 200nm~ 500nm。
The present invention does not have the concrete mode of the oxidation special restriction, using oxidation well known to those skilled in the art Mode preferably carries out autoxidation in air in the present invention.
The present invention provides a kind of N ions (N3-) doping CeO2The preparation method of film, in Ar and N2Mixed atmosphere in, Using metal Ce as target, CeN films are obtained through magnetron sputtering deposition, by CeN film oxidations obtained to get N3-Adulterate CeO2It is thin Film.N has been made using magnetron sputtering, physical gas-phase deposite method simultaneously in the present invention under cryogenic3-Adulterate CeO2Solid oxygen Compound fuel-cell electrolyte film overcomes ring caused by need to using high temperature and organic solvent using chemical preparation process in the past Border pollution problem, and compared with traditional chemical routes have prepare material homogeneity it is good, thickness controllable precise, jail is combined with substrate Gu, the advantages that nano-crystal film, N obtained can be prepared3-Adulterate CeO2N in film3-Ion maximum doping can reach 6.46%, N3-It is doped to CeO2Middle replacement part O2-Ion can improve O2-Ionic vacancies concentration, and then improve N3-Doping CeO2The ionic conductivity of solid-oxide fuel battery electrolyte film.
With reference to embodiment to N provided by the invention3-Adulterate CeO2The preparation method of film is described in detail, but It is that they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Metal Ce is put in as sputtering target material on radio frequency cathode, waits for that the background pressure of vacuum chamber reaches 9.5 × 10-5When Pa, It is passed through Ar gas and N simultaneously toward vacuum chamber2Gas, gas flow are controlled respectively in 30cm3/ point and 5cm3/ point, sputtering pressure control exists 0.8Pa, radio-frequency power 50W, carry out magnetron sputtering 2 hours at 25 DEG C, obtain CeN films.
Above-mentioned CeN films are taken out in vacuum chamber be placed in air and carry out autoxidation, obtain N3-Adulterate CeO2Film, The XRD diagram of film sample when oxidization time is 6 minutes, 8 hours, 15 hours and 2 days is measured respectively, and test results are shown in figure 1. From figure 1 it appears that when oxidization time is 6 minutes, the diffraction maximum of CeN phases sees also to be perfectly clear, and illustrates film at this time Sample not yet aoxidizes completely, and with the extension of oxidization time, the trend that film sample aoxidizes is more obvious, works as oxidation When time is 2 day time, the presence of CeN phases is not observed in XRD diffraction maximums at all, illustrates 2 days rear film samples by oxygen The comparison of change is abundant.
It whether there is N ions in the film sample after oxidation to verify, X carried out to the film sample after the oxidation Ray photoelectron spectroscopic analysis (XPS), the specifically film to film sample surface and through Ar ion etchings after ten minutes respectively Sample is tested, and the results are shown in Figure 2, as seen from Figure 2, does not detect trace existing for N ions on film sample surface Mark, but film sample internal detection has arrived N3-Existing signal illustrates that film sample at this time is N3-The CeO of doping type2Film, XPS test results show N3-Maximum doping can reach 6.46%.
Fig. 3 (a) is the N ion dopings CeO being deposited on single crystal Si substrate2The surface scan electron microscope of film, Fig. 3 (b) To be deposited on the N ion dopings CeO on single crystal Si substrate2The cross-sectional scans electron microscope of film, as seen from Figure 3, embodiment 1 N ion dopings CeO obtained2Uniformity of film is good, thickness controllable precise, is firmly combined with substrate.
Embodiment 2
Metal Ce is put in as sputtering target material on radio frequency cathode, waits for that the background pressure of vacuum chamber reaches 2.0 × 10-4When Pa, It is passed through Ar gas and N simultaneously toward vacuum chamber2Gas, gas flow are controlled respectively in 60cm3/ point and 10cm3/ point, sputtering pressure control exists 2Pa, radio-frequency power 200W, magnetron sputtering 4 hours at 200 DEG C, obtain CeN films.
Taken out in vacuum chamber above-mentioned CeN films be placed in air carry out room temperature autoxidation obtain N after 20 days3-Doping CeO2Film.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (2)

1. a kind of preparation method of N ion dopings thin film of ceria, includes the following steps：
(1) in Ar and N2Mixed atmosphere in, using metal Ce as target, CeN films are obtained through magnetron sputtering；
(2) by CeN film oxidations made from the step (1) to get N ion dopings CeO2Film；
The sputtering pressure of magnetron sputtering is 0.8~2.0Pa in the step (1)；
The radio-frequency power of magnetron sputtering is 50~200W in the step (1)；
The time of magnetron sputtering is 2~4 hours in the step (1)；
The temperature of magnetron sputtering is 25~200 DEG C in the step (1)；
The gas flow of Ar is 30~60cm in the step (1)3/ min, the N2Gas flow be 5~10cm3/min；
The pressure of vacuum chamber is 9.5 × 10 when the magnetron sputtering-5~2.0 × 10-4Pa；
Oxidation carries out in air in the step (2)；
The time aoxidized in the step (2) is 2 days~30 days；
The temperature aoxidized in the step (2) is 20~25 DEG C.
2. preparation method according to claim 1, which is characterized in that the lining used when magnetron sputtering in the step (1) Bottom is single crystalline Si.
CN201710427185.8A 2017-06-08 2017-06-08 A kind of preparation method of N ion dopings thin film of ceria Active CN107164728B (en)

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