CN105671486A - Preparation method of nitrogen-doped titanium dioxide film materials - Google Patents
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- CN105671486A CN105671486A CN201610180065.8A CN201610180065A CN105671486A CN 105671486 A CN105671486 A CN 105671486A CN 201610180065 A CN201610180065 A CN 201610180065A CN 105671486 A CN105671486 A CN 105671486A
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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
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- 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
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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
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- C23C14/48—Ion implantation
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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
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Abstract
The invention relates to a preparation method of nitrogen-doped titanium dioxide film materials, belonging to the fields of surface processing and coatings. The preparation method comprises the step of doping and injecting a nitrogen element on the surface of a titanium dioxide film by using a nitrogen ion beam to obtain the nitrogen-doped titanium dioxide film materials, wherein the crystal structure of the titanium dioxide film is a non-crystal structure, a polycrystal structure or a non-crystal and polycrystal mixed structure. The preparation method has the beneficial effects that parameters such as the crystallization degree and doping and injecting time of the titanium dioxide film material are regulated, so that nitrogen-doped titanium dioxide film materials with different nitrogen element doping amounts and states are prepared, and the controllability of the nitrogen element doping amounts and states is realized.
Description
Technical field
The present invention relates to the preparation method of a kind of nitrogen-doped titanium dioxide thin-film material, belong to surface working, coatings art.
Background technology
Nitrogen-doped titanium dioxide thin-film material is the important n-type semiconductor functional materials of a class, has important application in opto-electronic conversion field, such as solar battery light anode, visible light catalyst and photo-sensor etc. In recent years, N-TiO2In thin-film material preparation process N source selection and to N-TiO2In thin-film material, the control of N element dopant states more and more causes the concern of people, such as N-TiO2Ti-N key and the control of Ti-ON key doping ratio in thin-film material, both N(Ti-N)And N(Ti-ON)Ratio control. Consider N-TiO2The base material of thin-film material when opto-electronic conversion field is applied, building-up process requiring, synthesis temperature is requirement to doped element stability under room temperature and actual application environment, at TiO2In thin-film material process of growth, direct N is melted into as preparation N-TiO2The best approach of thin-film material. But, owing to other elements, Nization temperature height, N element doping and the reason such as doped difficulty control, the N element difficult control of stably-doped property are contained in N source, under practical service environment, N-TiO can be caused2N element loss or the doped change of N element in thin-film material, and then cause N-TiO2Thin-film material lost efficacy.
At present, different N source is utilized to prepare N-TiO2The method of material has: the people such as M.J.Powell (J.PhotochemistryandPhotobiologyA:Chemistry, 2014, Vol.281:27-34) are that N source utilizes sol-gel method to prepare N-TiO taking Tetramethyl Ethylene Diamine2Material; The people such as I.Ruzybayev (MaterialsScienceinSemiconductorProcessing, 2015, Vol.39:371-376) are with N2For N source utilizes pulsed laser deposition to prepare N-TiO2Material; The people such as S.Cao (AppliedSurfaceScience, 2014, Vol.309:119-127) are with N2For N source utilizes reactive magnetron sputtering method to prepare N-TiO2Film; The people such as M.Dawson (J.SolidStateChemistry, 2014, Vol.215:211-218) are with urea and N2For N source utilizes atmosphere sintering method to prepare N-TiO2Material; The people such as R.Quesada-Cabrera (AppliedCatalysisB:Environmental, 2014, Vol.160-161:582-588) are that N source utilizes atmospheric chemical vapor deposition to prepare N-TiO taking TERTIARY BUTYL AMINE2Film.
But, aforesaid method all comes with some shortcomings part, as: if preparing N-TiO with atmosphere sintering method2, there is temperature of reaction too high in thin-film material, easily destroys the base material of non-refractory, such as organic polymer material etc., there is the problems such as length consuming time, efficiency are low simultaneously; If preparing N-TiO with reactive magnetron sputtering method2, there is growth velocity slow in thin-film material, the problem such as the difficult control of N, O ratio in reactive sputtering process; If preparing N-TiO with pulse laser method2, there is the problems such as laser beam spot is little, efficiency is low, irradiation surface difficult control of temperature in thin-film material; If preparing N-TiO with sol-gel method2, there is N-TiO in thin-film material2Thin-film material surface roughness is big, surface exists the problems such as a large amount of random cracks.
Summary of the invention
N element doping is injected TiO by N ionic fluid by the present invention at ambient temperature2Film surface, to realize N element at TiO2Doping chemistry state in film is controlled, solves the problems referred to above.
The present invention provides the preparation method of a kind of nitrogen-doped titanium dioxide thin-film material, and described preparation method, for utilizing nitrogen ion beam that nitrogen-doping is injected titanium deoxid film surface, obtains nitrogen-doped titanium dioxide thin-film material;
The crystalline structure of described titanium deoxid film is non-crystalline substance, polycrystalline or non-crystalline substance and the mixing of polycrystalline.
The temperature that doping of the present invention is injected is preferably room temperature.
The distance on nitrogen ion beam of the present invention and titanium deoxid film surface is preferably 5-15cm.
Nitrogen ion beam of the present invention is preferably perpendicular to titanium deoxid film surface.
The time that doping of the present invention is injected is preferably 5-20min.
The ion source power density of generation nitrogen ion beam of the present invention is preferably 0.5-4.0W/cm2。
The ion source anode voltage of generation nitrogen ion beam of the present invention is preferably 500-3500V.
The working gas of nitrogen ion beam of the present invention is preferably high-purity N2。
Nitrogen-doping amount of the present invention is preferably 3-15at.%.
Nitrogen-doping state of the present invention is preferably N(Ti-N)Doping and N(Ti-ON)The mixing of doping, more preferably N(Ti-N)Doping and N(Ti-ON)The ratio of doping is 0.5-2:1.
The useful effect of the present invention is:
1. the present invention is by regulating the crystallization degree of titanium dioxide film materials, the parameters such as injection time of adulterating, prepare the nitrogen-doped titanium dioxide thin-film material and there is different nitrogen-doping amount and dopant states, it is achieved the controllable of nitrogen-doping amount and dopant states.
2. the working gas of nitrogen ion beam of the present invention is high-purity N2, pollution-free, can directly be discharged in air.
3. N doping method of the present invention is simple, cost is low, product rate height, be convenient to large-scale industrial production.
Accompanying drawing explanation
Accompanying drawing 7 width of the present invention,
Fig. 1 is the X ray diffracting spectrum of the titanium dioxide film materials that embodiment 1-5 obtains;
Fig. 2 is nitrogen ion beam using emission spectrum for diagnosing collection of illustrative plates in embodiment 1-5, wherein: Fig. 2 (a) is the emmission spectrum in 300-800nm interval, the interior illustration of Fig. 2 (a) is nitrogen molecule rotational spectrum, the partial enlargement figure that Fig. 2 (b) is Fig. 2 (a);
Fig. 3 is high resolution x-ray photoelectron energy spectrogram and the Gauss curve fitting graphic representation of the nitrogen element 1s orbital electron of the titanium deoxid film that embodiment 1 obtains;
Fig. 4 is high resolution x-ray photoelectron energy spectrogram and the Gauss curve fitting graphic representation of the nitrogen element 1s orbital electron of the titanium deoxid film that embodiment 2 obtains;
Fig. 5 is high resolution x-ray photoelectron energy spectrogram and the Gauss curve fitting graphic representation of the nitrogen element 1s orbital electron of the titanium deoxid film that embodiment 3 obtains;
Fig. 6 is high resolution x-ray photoelectron energy spectrogram and the Gauss curve fitting graphic representation of the nitrogen element 1s orbital electron of the titanium deoxid film that embodiment 4 obtains;
Fig. 7 is high resolution x-ray photoelectron energy spectrogram and the Gauss curve fitting graphic representation of the nitrogen element 1s orbital electron of the titanium deoxid film that embodiment 5 obtains.
Embodiment
Following non-limiting example can make the those of ordinary skill of this area more fully understand the present invention, but does not limit the present invention in any way.
Embodiment 1
The N doped Ti O that a kind of N dopant states is controlled2The preparation method of thin-film material, described preparation method comprises the steps:
1. DC pulse reaction magnetocontrol sputtering method is utilized at ambient temperature taking polyethylene terephthalate and quartz plate as base material, taking high pure metal Ti target (99.99%) as sputtering target material, taking high-purity Ar (99.99%) as sputter gas, with high-purity O2(99.99%) it is reactant gases, carries out Ar/O2Cosputtering mode prepares TiO2Film, the TiO obtained2Film thickness is 300nm, and energy gap is 3.32eV, and crystalline structure is non-crystal structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply operating frequency is 200kHz, power is 150W, Ar flow is 20sccm, O2Flow is 4sccm, and back end vacuum tightness is 3.0 × 10-3Pa, sputtering vacuum tightness is 0.7Pa, and depositing time is 720min.
2. the N ionic fluid utilizing Kao Fuman type ion source to produce is perpendicular to the step 1. surperficial implantation step 1. products obtained therefrom surface of N element being adulterated of products obtained therefrom at ambient temperature, the distance on N ionic fluid and step 1. products obtained therefrom surface is 9cm, the time that doping is injected is 5min, and ion source power density is 1.07W/cm2, ion source anode voltage is the working gas of 1451V, N ionic fluid is high-purity N2(99.99%), as shown in Figure 2, non-brilliant TiO is injected in the doping of N ionic fluid to N ionic fluid using emission spectrum for diagnosing collection of illustrative plates2N-TiO is formed after film surface2Film, N-TiO2Film energy gap is reduced to 3.15eV, N-TiO2In film, N element doping is 13.9at.%, and N element chemical bonding structure is Ti-N key and the mixing of Ti-ON key, and its chemical state in chemical bonding structure is respectively N(Ti-N)With N(Ti-ON), and N(Ti-N): N(Ti-ON)=0.51:1, as shown in Figure 3.
Embodiment 2
The N doped Ti O that a kind of N dopant states is controlled2The preparation method of thin-film material, described preparation method comprises the steps:
1. Radiofrequency muti-hook probe method is utilized at ambient temperature taking single crystalline Si (100) substrate and quartz plate as base material, with high pure metal TiO2Target (99.99%) is sputtering target material, taking high-purity Ar (99.99%) as sputter gas, with high-purity O2(99.99%) it is reactant gases, carries out Ar/O2Cosputtering mode prepares TiO2Film, the TiO obtained2Film thickness is 300nm, and energy gap is 3.22eV, and crystalline structure is non-crystal structure, as shown in Figure 1;
Wherein: wave packet shielding power supply operating frequency is 13.56MHz, power is 400W, Ar flow is 19sccm, O2Flow is 1sccm, and back end vacuum tightness is 2.0 × 10-3Pa, sputtering vacuum tightness is 0.6Pa, and depositing time is 180min.
2. the N ionic fluid utilizing Kao Fuman type ion source to produce is perpendicular to the step 1. surperficial implantation step 1. products obtained therefrom surface of N element being adulterated of products obtained therefrom at ambient temperature, the distance on N ionic fluid and step 1. products obtained therefrom surface is 15cm, the time that doping is injected is 10min, and ion source power density is 2.86W/cm2, ion source anode voltage is the working gas of 2185V, N ionic fluid is high-purity N2(99.99%), as shown in Figure 2, non-brilliant TiO is injected in the doping of N ionic fluid to N ionic fluid using emission spectrum for diagnosing collection of illustrative plates2N-TiO is formed after film surface2Film, N-TiO2Film energy gap is reduced to 3.14eV, N-TiO2In film, N element doping is 12.5at.%, and N element chemical bonding structure is Ti-N key and the mixing of Ti-ON key, and its chemical state in chemical bonding structure is respectively N(Ti-N)With N(Ti-ON), and N(Ti-N): N(Ti-ON)=0.59:1, as shown in Figure 4.
Embodiment 3
The N doped Ti O that a kind of N dopant states is controlled2The preparation method of thin-film material, described preparation method comprises the steps:
1. DC pulse reaction magnetocontrol sputtering method is utilized at ambient temperature taking common slide glass and quartz plate as base material, taking high pure metal Ti target (99.99%) as sputtering target material, taking high-purity Ar (99.99%) as sputter gas, with high-purity O2(99.99%) it is reactant gases, carries out Ar/O2Cosputtering mode prepares TiO2Film, the TiO obtained2Film thickness is 300nm, and energy gap is 3.19eV, and crystalline structure is polycrystalline anatase octahedrite phase structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply operating frequency is 150kHz, power is 900W, Ar flow is 16sccm, O2Flow is 4sccm, and back end vacuum tightness is 2.0 × 10-3Pa, sputtering vacuum tightness is 0.6Pa, and depositing time is 54min.
2. the N ionic fluid utilizing Kao Fuman type ion source to produce is perpendicular to the step 1. surperficial implantation step 1. products obtained therefrom surface of N element being adulterated of products obtained therefrom at ambient temperature, the distance on N ionic fluid and step 1. products obtained therefrom surface is 10cm, the time that doping is injected is 20min, and ion source power density is 1.10W/cm2, ion source anode voltage is the working gas of 1420V, N ionic fluid is high-purity N2(99.99%), as shown in Figure 2, polycrystalline anatase octahedrite TiO is injected in the doping of N ionic fluid to N ionic fluid using emission spectrum for diagnosing collection of illustrative plates2N-TiO is formed after film surface2Film, N-TiO2Film energy gap is reduced to 3.11eV, N-TiO2In film, N element doping is 6.6at.%, and N element chemical bonding structure is Ti-N key and the mixing of Ti-ON key, and its chemical state in chemical bonding structure is respectively N(Ti-N)With N(Ti-ON), and N(Ti-N): N(Ti-ON)=0.81:1, as shown in Figure 5.
Embodiment 4
The N doped Ti O that a kind of N dopant states is controlled2The preparation method of thin-film material, described preparation method comprises the steps:
1. DC pulse reaction magnetocontrol sputtering method is utilized at ambient temperature taking single crystalline Si (100) substrate and quartz plate as base material, taking high pure metal Ti target (99.99%) as sputtering target material, taking high-purity Ar (99.99%) as sputter gas, with high-purity O2(99.99%) it is reactant gases, carries out Ar/O2Cosputtering mode prepares TiO2Film, the TiO obtained2Film thickness is 300nm, and energy gap is 3.32eV, and crystalline structure is non-crystal structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply operating frequency is 200kHz, power is 450W, Ar flow is 16sccm, O2Flow is 4sccm, and back end vacuum tightness is 2.0 × 10-3Pa, sputtering vacuum tightness is 0.6Pa, and depositing time is 200min.
2. by step 1. products obtained therefrom put into retort furnace and carry out air atmosphere annealing, annealing parameter is: temperature rise rate is 5 DEG C/min, annealing temperature is 600 DEG C, soaking time is 60min, the temperature fall time being at the uniform velocity cooled to 100 DEG C by 600 DEG C is 12h, the temperature fall time being at the uniform velocity cooled to room temperature by 100 DEG C is 1h, the TiO obtained2Film energy gap is 3.17eV, and crystalline structure is polycrystalline anatase octahedrite phase structure, as shown in Figure 1.
3. the N ionic fluid utilizing Kao Fuman type ion source to produce is perpendicular to the step 2. surperficial implantation step 2. products obtained therefrom surface of N element being adulterated of products obtained therefrom at ambient temperature, the distance on N ionic fluid and step 2. products obtained therefrom surface is 10cm, the time that doping is injected is 20min, and ion source power density is 1.10W/cm2, ion source anode voltage is the working gas of 1430V, N ionic fluid is high-purity N2(99.99%), as shown in Figure 2, polycrystalline anatase octahedrite TiO is injected in the doping of N ionic fluid to N ionic fluid using emission spectrum for diagnosing collection of illustrative plates2N-TiO is formed after film surface2Film, N-TiO2Film energy gap is reduced to 2.97eV, N-TiO2In film, N element doping is 7.9at.%, and N element chemical bonding structure is Ti-N key and the mixing of Ti-ON key, and its chemical state in chemical bonding structure is respectively N(Ti-N)With N(Ti-ON), and N(Ti-N): N(Ti-ON)=1.56:1, as shown in Figure 6.
Embodiment 5
The N doped Ti O that a kind of N dopant states is controlled2The preparation method of thin-film material, described preparation method comprises the steps:
1. it is solvent taking dehydrated alcohol, taking oleic acid and polyvinylpyrrolidone as dispersion agent, with P25 type nano-TiO2Powder body is solute configuration slurry, is base material taking quartz plate, utilizes spin-coating method to revolve in quartz plate substrate and is coated with TiO2Film, the TiO obtained2Film thickness is 500nm, and energy gap is 3.18eV, and crystalline structure is polycrystalline, and is anatase octahedrite phase and the duplex grain structure of rutile phase, as shown in Figure 1;
Wherein: the volumn concentration of oleic acid is the 0.5% of solvent, the volumn concentration of polyvinylpyrrolidone is 0.5%, P25 type nano-TiO of solvent2The mass percentage of powder body is the 5% of solvent, and quartz plate substrate speed of rotation is 2000 turns/min, and drying temperature is 150 DEG C, and time of drying is 10min, revolves and is coated with after 5 times first drying and calcines 10min under 500 DEG C of air conditionses again.
2. the N ionic fluid utilizing Kao Fuman type ion source to produce is perpendicular to the step 1. surperficial implantation step 1. products obtained therefrom surface of N element being adulterated of products obtained therefrom at ambient temperature, the distance on N ionic fluid and step 1. products obtained therefrom surface is 5cm, the time that doping is injected is 20min, and ion source power density is 1.10W/cm2, ion source anode voltage is the working gas of 1470V, N ionic fluid is high-purity N2(99.99%), as shown in Figure 2, polycrystalline and anatase octahedrite phase and rutile phase mixed crystal TiO are injected in the doping of N ionic fluid to N ionic fluid using emission spectrum for diagnosing collection of illustrative plates2N-TiO is formed after film surface2Film, N-TiO2Film energy gap is reduced to 3.09eV, N-TiO2In film, N element doping is 6.2at.%, and N element chemical bonding structure is Ti-N key and the mixing of Ti-ON key, and its chemical state in chemical bonding structure is respectively N(Ti-N)With N(Ti-ON), and N(Ti-N): N(Ti-ON)=0.90:1, as shown in Figure 7.
Claims (6)
1. the preparation method of a nitrogen-doped titanium dioxide thin-film material, it is characterised in that: described preparation method, for utilizing nitrogen ion beam that nitrogen-doping is injected titanium deoxid film surface, obtains nitrogen-doped titanium dioxide thin-film material;
The crystalline structure of described titanium deoxid film is non-crystalline substance, polycrystalline or non-crystalline substance and the mixing of polycrystalline.
2. preparation method according to claim 1, it is characterised in that: the temperature that described doping is injected is room temperature.
3. preparation method according to claim 1, it is characterised in that: the distance on described nitrogen ion beam and titanium deoxid film surface is 5-15cm.
4. preparation method according to claim 1, it is characterised in that: the time that described doping is injected is 5-20min.
5. preparation method according to claim 1, it is characterised in that: the ion source power density of described generation nitrogen ion beam is 0.5-4.0W/cm2。
6. preparation method according to claim 1, it is characterised in that: the ion source anode voltage of described generation nitrogen ion beam is 500-3500V.
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| CN107774289A (en) * | 2016-08-29 | 2018-03-09 | 中国科学院福建物质结构研究所 | A kind of photocatalytic cleavage water hydrogen manufacturing film catalyst and its preparation method and application |
| CN112427044A (en) * | 2019-08-26 | 2021-03-02 | 中国科学院上海硅酸盐研究所 | Nitrogen-doped mixed-crystal titanium dioxide photocatalytic material and preparation method and application thereof |
| TWI818610B (en) * | 2022-06-30 | 2023-10-11 | 國立中興大學 | Photoelectrochemical device |
| TWI820777B (en) * | 2022-06-30 | 2023-11-01 | 國立中興大學 | Photoelectrochemical device |
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| TWI820777B (en) * | 2022-06-30 | 2023-11-01 | 國立中興大學 | Photoelectrochemical device |
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