CN102294234A - Composite titanium dioxide photocatalyst and preparation method thereof - Google Patents
Composite titanium dioxide photocatalyst and preparation method thereof Download PDFInfo
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Abstract
The invention provides a composite titanium dioxide photocatalyst. The composite titanium dioxide photocatalyst comprises an inert metal micro/nano-structure, a diamond-like carbon film deposited on the inert metal micro/nano-structure, and nano-titanium dioxide coated outside the diamond-like carbon film, wherein the thickness of the diamond-like carbon film is in a range of 1 to 2 nanometers. In the invention, the diamond-like carbon film which is ultra-thin is coated on the inert metal micro/nano-structure to prevent that photo-generated electrons of titanium dioxide are transferred to a metal, and thus a surface plasmon polariton effect of the inert metal micro/nano-structure is stimulated and an enhanced electric field is generated and is stronger than an electric field generated by a pure metal micro/nano-structure so that titanium dioxide photocatalytic efficiency is improved greatly. Therefore, the composite titanium dioxide photocatalyst can be utilized widely for removal of indoor pollutants, sterilization and degradation of organic dye pollutants.
Description
Technical field
The present invention relates to a kind of composite titanium dioxide photochemical catalyst, relate in particular to a kind of DLC film clad metal micro-nano structure/TiO
2Type composite photo-catalyst and preparation method thereof.
Background technology
Surface phasmon is meant the electromagnetic wave of propagating along the metal surface in the free electron of metal surface existence and photon interaction generation, and its direction of propagation then is the index decay along the medium/metal surface in the vertical interface direction.In recent years, maturation along with nanometer technology, metal micro-nanostructure is owing to forming the electromagnetic field that local strengthens near the spatial dimension of the light local nanoscale metal surface, with respect to incident field, the electromagnetic field intensity that local strengthens can reach more than 100 times, the efficient of many two-phonon process is significantly improved, and this is that additive method is beyond one's reach, and therefore is subjected to extensive concern and research.Metal micro-nanostructure is at TiO
2Application during photocatalysis efficiency improves is exactly a case history.
Japanese Fujishima found TiO from 1972
2After can carrying out the photolysis reactions of water as electrode, just caused and utilized semiconductor light-catalyst luminous energy to be converted into the research boom of electric energy and chemical energy.TiO
2Utilize luminous energy to drive redox reaction, utilize self strong oxidability can carry out organic decomposition reaction, thereby have photocatalytic activity, be widely used in the removal of environmental protection and chemical pollutant.In addition, microbial bacterial is to be made of organic compound, therefore can utilize TiO
2Photocatalysis removed extremely.General commonly used bactericide such as silver etc. can make cell lose activity, but after bacterium is killed, can discharge pyrogenicity and poisonous component such as endotoxin, TiO
2Photochemical catalyst can not only killing bacteria, and the toxic compounds that can degrade simultaneously and be discharged by bacterium.The clear professor in island that rises of Tokyo University engineering portion waits proof TiO
2Pseudomonas aeruginosa, Escherichia coli and staphylococcus aureus etc. there is very strong sterilizing ability.Therefore, based on TiO
2The type photochemical catalyst is widely used in indoor air purification, dyestuff contaminant removal and degerming etc.
TiO
2The degradation principles of type photochemical catalyst is based on and produces electron-hole pair under the illumination condition, the valence band hole is good oxidant, conduction band electron is a better reductant, oxygen around electronics and hole make and hydrone are excited into has active free ion bases such as OH, and these ion radicals can decompose human body or the harmful organic substance of environment.In photocatalysis, the hole has bigger reactivity, and degradable organic pollutant is played a major role.
For TiO
2The type photochemical catalyst, how improving its efficient is the problem in science of a key in using at present, international at present and domestic a lot of people has carried out extensive studies to this.At first from TiO
2The degradation principles of type photochemical catalyst, how to reduce the compound of electronics and hole, be to improve one of photocatalysis efficiency efficient ways, main at present employing metal ion or other semi-conducting materials mix, these doping can become the trap in electronics or hole and prolong life-span of OH free radical, thereby improve photocatalysis efficiency effectively, but shortcoming is metal-doped TiO
2Unstable.Another one method effectively is to adopt the surface phasmon electric field of metal micro-nanostructure to strengthen, cardinal principle is to utilize incident light to excite the surface phasmon of metal micro-nanostructure, producing very strong electric field strengthens, and the electric field of this enhancing can gain near two-phonon process, promptly improves TiO
2Efficiency of light absorption, more electron hole pair is provided.K.Awazu (K.Awazu, M.Fujimaki, C.Rockstuhl et al, J.Am.Chem.Soc.2008,130,1676) etc. utilizes this effect to obtain the photocatalysis efficiency higher than metal ion mixing.Strengthen TiO at metal micro-nanostructure
2Photocatalysis efficiency the time, mainly be utilize to absorb to strengthen, rather than stop the compound of electron-hole pair, because metal micro-nanostructure is directly and TiO
2Contact is because the work function of metal is higher than TiO
2Work function, make electronics transfer to the metal surface, thereby suppress the generation that surface phasmon strengthens electric field.(comprise K.Awazu etc.) at present in the world and mainly adopt SiO
2Layer clad metal micro-nano structure realizes that electric field strengthens photocatalysis efficiency.Though adopt the method to obtain, also a lot of defectives than the better effect of conventional metals ion doping.At first, when adopting thicker dielectric layer to coat, the main local of largest portion that strengthens electric field is in dielectric layer, make the electric field ratio metallic surface electric field of dielectric layer outer surface decrease, how the highfield in the dielectric layer being discharged into the dielectric layer outer surface is to utilize metal micro-nanostructure to strengthen TiO
2The key scientific problems of photocatalysis efficiency.
Summary of the invention
The invention provides a kind of composite titanium dioxide photochemical catalyst and preparation method thereof, to overcome the above-mentioned defective that prior art exists.
The present invention realizes by the following technical solutions:
A kind of composite titanium dioxide photochemical catalyst, by the inert metal micro-nano structure, be deposited on the outer DLC film layer of described inert metal micro-nano structure, and being coated on the outer nano titanium oxide composition of described DLC film layer, the thickness of wherein said DLC film layer is 1~2 nanometer.
Described inert metal can be gold, silver, platinum, copper, and the size of microscopic particles or cluster structure is at nanometer or micron order, gold, silver, the platinum of preferred average grain diameter 10~150 nanometers, and described micro-nano structure is nanostructured and nano particle;
Described DLC film can be hydrogeneous amorphous carbon-film (a-C:H), also can be non-hydrogen amorphous film, for example a-C film or ta-C film, preferably tetrahedral amorphous carbon film or nitrogen, fluorine doping tetrahedral amorphous carbon film;
Described titanium dioxide can be fine and close film layer structure, also can be loose nano particle, and the crystalline structure of titanium dioxide is preferably the anatase phase.
The present invention also discloses a kind of method for preparing above-mentioned composite titanium dioxide photochemical catalyst, comprises the steps:
(1) fixing inert metal micro-nano structure on base material;
(2) deposit thickness is the DLC film layer of 1~2 nanometer on described inert metal micro-nano structure;
(3) clad nano titanium dioxide on described DLC film layer.
According to the practical application needs, step (1) can apply synthetic in advance inert metal micro-nano structure material and be fixed on substrate surface, also can adopt this area conventional method on base material, to deposit inert metal micro-nano structure substrate, for example elementide sputtering method, electron beam exposure, nano impression etc. preferably adopt the inert metal substrate of elementide sputtering method depositing nano structure on base material; It is standby that step (1) also can directly be selected synthetic in advance nanometer inert metal particle for use in addition;
Step (2) can adopt this area conventional method depositing diamond-like thin layer on the inert metal micro-nano structure, for example filtered cathodic vacuum arc method, chemical vapour deposition technique etc. preferably adopt the filtered cathodic vacuum arc method to deposit described DLC film layer;
Step (3) can adopt this area conventional method, and for example magnetron sputtering method depositing nano titanium deoxid film layer on the DLC film layer mainly is at inert metal nanostructured substrate; Also the inert metal particle of the DLC film layer coating that step (2) can be obtained is mixed in the nano TiO 2 powder and makes composite granule by stirring; Also the inert metal particle of the DLC film layer coating that step (2) can be obtained is injected in the colloidal tio 2 for preparing, and then colloid mixture is loaded on the base material, 350~550 ℃ of annealing down, obtains the titanium deoxid film of anatase structures.
Described base material is glass or ceramic material, the preferred glass base material.
The present invention adopts the method for ultrathin diamond film clad metal structure, finds that unexpectedly it can greatly improve optically catalytic TiO 2 efficient.This may be because when the thickness of DLC film was reduced to 1~2 nanometer, its fine and close structure can stop the transfer of electronics, thus the generation of induced nano metal structure surface phasmon electric field; Secondly, because diamond thin is thinner, it is not enough to highfield is strapped in the so thin dielectric layer, can obtain stronger electric field enhancing at the dielectric layer outer surface on the contrary.
The inventor further discovers, thickening along with DLC film, be index like decay because the loss of scattering-in light and surface plasmon resonance electric field leave the surface, the surface field of the feasible substrate of modifying with respect to the substrate of unmodified reduced; When the inventor finds that thickness when DLC film is greater than 1 nanometer and less than 2 nanometers, can stop electronics to transfer to metal effectively, and demonstrate stronger electric field enhancing than the metal of unmodified.If but the thickness of DLC film less than 1 nanometer, the then DLC film discontinuous densification that becomes can't stop electronics to be transferred on the metal, cause can't induced nano metal structure surface phasmon electric field generation, just do not have the electric field of enhancing yet and can not use.
A kind of DLC film clad metal micro-nano structure/TiO of the present invention
2The type photochemical catalyst is compared with prior art and is had the following advantages:
1, because ultrathin diamond film clad nano inert metal of the present invention not only can stop TiO
2Light induced electron transfer on the metal, and can excite the surface phasmon effect of metal micro-nanostructure to obtain the enhancing electric field stronger, thereby realize maximum TiO than simple metal micro-nanostructure
2Photocatalysis efficiency improves.
2, a kind of DLC film clad metal micro-nano structure/TiO of the present invention
2The type photochemical catalyst, applied widely, at different TiO
2Preparation method and different TiO
2Structure can be selected different metals, as gold, silver, platinum etc.; Simultaneously at different TiO
2As particle or film, also can select different metal micro-nanostructures such as metal Nano structure or nano particle for use.
3, a kind of DLC film clad metal micro-nano structure/TiO of the present invention
2The type photochemical catalyst can be widely used in the degraded of indoor pollutant removal, sterilization and organic dye pollutant.
4, DLC film clad metal micro-nano structure/TiO provided by the invention
2The preparation method of type photochemical catalyst, wherein ultrathin diamond thin film technique maturation, production cost are low, can realize industrialized production.
Description of drawings
Fig. 1 is the comparing result figure that the amorphous carbon film of different-thickness coats Ag nanocluster structure/TiO2 type photocatalyst for degrading methylene blue.
Fig. 2 removes colibacillary comparing result figure for DLC film coats platinum nanocluster structure/TiO2 type photochemical catalyst.
Fig. 3 is that the amorphous carbon film of different-thickness coats Ag nano particle/TiO
2The comparing result figure of type photocatalytic degradation methylene blue.
The specific embodiment
Provide preferred embodiment of the present invention below in conjunction with accompanying drawing, to describe technical scheme of the present invention in detail.
A kind of based on DLC film coated with silver nanocluster structure/TiO
2The preparation method of type photochemical catalyst:
(1) adopt elementide sputter deposition (with reference to Chinese patent CN101482528 disclosed method) on glass substrate, to prepare the substrate of the banking group clustering architecture of average grain diameter 50 nanometers.
(2) the tetrahedral amorphous carbon film of employing filtered cathodic vacuum arc method deposit thickness 1 nanometer on the substrate of the Nano Silver cluster structure that step (1) prepares.Finish (with reference to disclosed method among the Chinese patent CN1235695A) on the FCVA origin system that the filtered cathodic vacuum arc method adopts Singapore Nanofilm Technologies Internat to produce.
(3) adopt magnetically controlled sputter method (reference literature Materials Research Bulletin 46,52 (2011) described methods) depositing Ti O on the Nano Silver cluster structured substrate that the ultrathin diamond film that step (2) prepares coats
2Film 50 nanometers are annealed down at 350 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Embodiment 2
The tetrahedral amorphous carbon film thickness that deposits on the substrate of Nano Silver cluster structure except that step (2) is 1.5 nanometers, and other steps are with embodiment 1.
Embodiment 3
The tetrahedral amorphous carbon film thickness that deposits on the substrate of Nano Silver cluster structure except that step (2) is 2 nanometers, and other steps are with embodiment 1.
Comparative Examples 1
The tetrahedral amorphous carbon film thickness that deposits on the substrate of Nano Silver cluster structure except that step (2) is 4 nanometers, and other steps are with embodiment 1.
Comparative Examples 2
The preparation of simple titanium deoxid film: adopt magnetically controlled sputter method direct depositing Ti O on glass substrate
2Film 50 nanometers are annealed down at 350 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Comparative Examples 3
Do not coat the preparation of the Nano Silver cluster structure/TiO2 film-type photochemical catalyst of amorphous carbon film layer:
(1) adopt the elementide sputter deposition on glass substrate, to prepare the substrate of the banking group clustering architecture of average grain diameter 50 nanometers;
(2) adopt magnetically controlled sputter method direct depositing Ti O on the Nano Silver cluster structured substrate that step (1) prepares
2 Film 50 nanometers are annealed down at 350 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Embodiment 4
A kind of based on DLC film coating platinum nanocluster structure/TiO
2The preparation method of type photochemical catalyst:
(1) adopt the elementide sputter deposition on glass substrate, to prepare the substrate of the platinum cluster structure of average grain diameter 130 nanometers.
(2) the tetrahedral amorphous carbon film of employing filtered cathodic vacuum arc method deposit thickness 1 nanometer on the substrate of the nanometer platinum cluster structure that step (1) prepares.Finish on the FCVA origin system that the filtered cathodic vacuum arc method adopts Singapore Nanofilm Technologies Internat to produce.
(3) adopt magnetically controlled sputter method depositing Ti O on the nanometer platinum cluster structured substrate that the ultrathin diamond film that step (2) prepares coats
2Film 45 nanometers are annealed down at 450 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Comparative Examples 4
The preparation of simple titanium deoxid film: adopt magnetically controlled sputter method direct depositing Ti O on glass substrate
2Film 45 nanometers are annealed down at 450 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Comparative Examples 5
Do not coat the preparation of the nanometer platinum cluster structure/TiO2 film-type photochemical catalyst of amorphous carbon film layer:
(1) adopt the elementide sputter deposition on glass substrate, to prepare the substrate of the platinum cluster structure of average grain diameter 130 nanometers;
Adopt magnetically controlled sputter method direct depositing Ti O on the Nano Silver cluster structured substrate that step (1) prepares
2Film 45 nanometers are annealed down at 450 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Embodiment 5
A kind of based on DLC film coated with silver nano particle/TiO
2The preparation method of type photochemical catalyst:
(1) adopt chemical method (reference literature J.AM.CHEM.SOC.1676,130 (2008) disclosed methods) method to prepare the silver nano-grain of average grain diameter 50 nanometers;
(2) the tetrahedral amorphous carbon film of employing filtered cathodic vacuum arc method deposit thickness 1 nanometer on the silver nano-grain that step (1) prepares.Finish (with reference to disclosed method among the Chinese patent CN 1235695A) on the FCVA origin system that the filtered cathodic vacuum arc method adopts Singapore Nanofilm Technologies Internat to produce;
(3) adopt sol-gel process (with reference to Chinese patent CN1467024A disclosed method) preparation TiO
2Colloid, the Nano Silver nano particle that coats of the ultrathin diamond film that step (2) is prepared is incorporated into the TiO for preparing then
2In the colloid, on glass substrate, deposit one deck composite Ti O by czochralski method
2Colloid, thickness are 100 nanometers, and annealing down at 350 ℃ then obtains having the anatase phase TiO of high catalytic activity
2Film.
Embodiment 6
The tetrahedral amorphous carbon film thickness that deposits on nano-Ag particles except that step (2) is 1.5 nanometers, and other steps are with embodiment 1.
Embodiment 7
The tetrahedral amorphous carbon film thickness that deposits on nano-Ag particles except that step (2) is 2 nanometers, and other steps are with embodiment 1.
Comparative Examples 6
The tetrahedral amorphous carbon film thickness that deposits on nano-Ag particles except that step (2) is 4 nanometers, and other steps are with embodiment 1.
Comparative Examples 7
The preparation of simple titanium deoxid film: adopt sol-gel process (with reference to Chinese patent CN1467024A disclosed method) direct depositing Ti O on glass substrate
2Film 100 nanometers are annealed down at 350 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Comparative Examples 8
Do not coat the nano-Ag particles/TiO of amorphous carbon film layer
2The preparation of film-type photochemical catalyst:
(1) adopt chemical method (reference literature J.AM.CHEM.SOC.1676,130 (2008) disclosed methods) method to prepare the silver nano-grain of average grain diameter 50 nanometers;
(2) adopt sol-gel process (with reference to Chinese patent CN1467024A disclosed method) direct depositing Ti O on glass substrate
2Film 100 nanometers are annealed down at 350 ℃ then and are obtained having the anatase phase TiO of high catalytic activity
2Film.
Application Example 1
The substrate that embodiment 1~3 and Comparative Examples 1~3 are made is respectively put in the methylene blue solution of 0.01mmol/L, utilizes uviol lamp (wavelength 365 nanometers, 20 watts of power) irradiation, utilizes extinction spectrum to study its photocatalysis effect then, specifically sees Fig. 1.
The photocatalytic degradation experiment shows, Nano Silver cluster structured substrate/TiO that 1 nanometer DLC film coats
2Film-type photochemical catalyst photocatalysis effect is best, is simple TiO
2Seven times of film are the Nano Silver cluster structured substrate/TiO that do not coat
2Three times of film-type photochemical catalyst.
Application Example 2
On the substrate that embodiment 4 and Comparative Examples 4 and 5 make, cultivate Escherichia coli respectively, utilize uviol lamp (wavelength 365 nanometers, 20 watts of power) irradiation then,, specifically see Fig. 2 by the colibacillary removal situation of microscopic examination.
Escherichia coli are removed degradation experiment and show, nanometer platinum cluster structure/TiO that 1 nanometer DLC film coats
2Film-type photochemical catalyst bactericidal effect is best, is simple TiO
2About ten times of film, be the nanometer platinum cluster structure/TiO that does not coat
2About six times of the film-type photochemical catalyst.
Application Example 3
The substrate that embodiment 5~7 and Comparative Examples 6~8 are made is respectively put in the methylene blue solution of 0.01mmol/L, utilizes uviol lamp (wavelength 365 nanometers, 20 watts of power) irradiation, utilizes extinction spectrum to study its photocatalysis effect then, specifically sees Fig. 3.
The photocatalytic degradation experiment shows, nano-Ag particles/TiO that 1 nanometer DLC film coats
2Film-type photochemical catalyst photocatalysis effect is best, is simple TiO
2The twelvefold of film is the nano-Ag particles/TiO that does not coat
2Seven times of film-type photochemical catalyst.
Claims (8)
1. composite titanium dioxide photochemical catalyst, it is characterized in that, by the inert metal micro-nano structure, be deposited on the DLC film layer on the described inert metal micro-nano structure, and being coated on the outer nano titanium oxide composition of described DLC film layer, the thickness of wherein said DLC film layer is 1~2 nanometer.
2. composite titanium dioxide photochemical catalyst according to claim 1 is characterized in that, described inert metal micro-nano structure is the gold, silver or the platinum of average grain diameter 10~150 nanometers.
3. composite titanium dioxide photochemical catalyst according to claim 1 is characterized in that, described DLC film is tetrahedral amorphous carbon film or nitrogen, fluorine doping tetrahedral amorphous carbon film.
4. composite titanium dioxide photochemical catalyst according to claim 1 is characterized in that, described titanium dioxide is for being film and nano-powder particle, and crystal structure is the anatase phase.
5. a method for preparing as claim 1~4 composite titanium dioxide photochemical catalyst as described in each is characterized in that, comprises the steps:
(1) fixing inert metal micro-nano structure on base material;
(2) deposit thickness is the DLC film layer of 1~2 nanometer on described inert metal micro-nano structure;
(3) clad nano titanium dioxide on described DLC film layer.
6. method according to claim 5 is characterized in that, step (1) adopts the elementide sputtering method to deposit the nano-metal particle of described inert metal nanostructured substrate and chemical method preparation on base material, and described inert metal is gold, silver or platinum.
7. method according to claim 5 is characterized in that, step (2) adopts the filtered cathodic vacuum arc method to deposit described DLC film layer.
8. method according to claim 5 is characterized in that, the described nano titanium oxide form of step (3) is film or powder.
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CN102909008A (en) * | 2012-10-26 | 2013-02-06 | 湖北工业大学 | Preparation method for TiO2/SiO2-Ag-SiO2 nanocomposite film |
CN103736508A (en) * | 2013-12-26 | 2014-04-23 | 大连大学 | Method for preparing F-doped TiO2 by using atmospheric pressure plasma body |
CN105344342A (en) * | 2015-11-09 | 2016-02-24 | 复旦大学 | Photocatalyst environment purifying material based on active carbon and preparation method therefor |
CN106732571A (en) * | 2016-11-24 | 2017-05-31 | 杨健男 | Composite of anatase titanium dioxide and gold nanometer film and preparation method thereof |
WO2018152975A1 (en) * | 2017-02-22 | 2018-08-30 | 南方科技大学 | Photo-catalyst assembly and a preparation method therefor |
CN112233702A (en) * | 2020-10-26 | 2021-01-15 | 东北师范大学 | Preparation method and application of hydrogel-modified high-stability carbon-based holographic optical disk |
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CN102909008A (en) * | 2012-10-26 | 2013-02-06 | 湖北工业大学 | Preparation method for TiO2/SiO2-Ag-SiO2 nanocomposite film |
CN103736508A (en) * | 2013-12-26 | 2014-04-23 | 大连大学 | Method for preparing F-doped TiO2 by using atmospheric pressure plasma body |
CN105344342A (en) * | 2015-11-09 | 2016-02-24 | 复旦大学 | Photocatalyst environment purifying material based on active carbon and preparation method therefor |
CN106732571A (en) * | 2016-11-24 | 2017-05-31 | 杨健男 | Composite of anatase titanium dioxide and gold nanometer film and preparation method thereof |
CN106732571B (en) * | 2016-11-24 | 2019-04-19 | 杨健男 | The composite material and preparation method of anatase titanium dioxide and gold nanometer film |
WO2018152975A1 (en) * | 2017-02-22 | 2018-08-30 | 南方科技大学 | Photo-catalyst assembly and a preparation method therefor |
US11179699B2 (en) | 2017-02-22 | 2021-11-23 | Southern University Of Science And Technology | Photocatalytic assembly and its preparation method |
CN112233702A (en) * | 2020-10-26 | 2021-01-15 | 东北师范大学 | Preparation method and application of hydrogel-modified high-stability carbon-based holographic optical disk |
CN112233702B (en) * | 2020-10-26 | 2021-10-01 | 东北师范大学 | Preparation method and application of hydrogel-modified high-stability carbon-based holographic optical disk |
CN113937257A (en) * | 2021-08-27 | 2022-01-14 | 山东大学 | Nitrogen and fluorine co-doped titanium dioxide/carbon microsphere material, preparation method thereof and application thereof in sodium ion battery |
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Application publication date: 20111228 |