CN1962060A - Metal nano photocatalyst composite material and its preparation method - Google Patents
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Abstract
本发明涉及一种核壳型金属纳米光催化剂复合材料及其制法。该核壳型金属纳米光催化剂复合材料包含：一核心，为金属纳米粒子；一核壳，为二氧化钛纳米微粒。该复合材料的制造方法包含：首先形成一纳米粒径的二氧化钛粒子溶液，接着在该溶液中加入一同时具有第一官能团及第二官能团的多官能团化合物，该二氧化钛粒子是通过该第一官能团与该多官能团化合物反应相接，最后加入一金属纳米粒子与该第二官能团进行反应并结合。本发明所合成的核壳型金属纳米光催化剂复合材料可有效利用可见光，并具有分解甲醛、分解氮氧化物及抑菌的效果。此外，本发明的金属纳米光催化剂复合材料可提升光电池的转换效率。
The invention relates to a core-shell metal nano photocatalyst composite material and a preparation method thereof. The core-shell metal nano-photocatalyst composite material comprises: a core, which is metal nano particles; a core-shell, which is titanium dioxide nano particles. The manufacturing method of the composite material comprises: first forming a solution of titanium dioxide particles with a nanometer particle size, and then adding a multifunctional compound having both a first functional group and a second functional group to the solution, and the titanium dioxide particles are formed through the first functional group and the second functional group. The multifunctional compound reacts successively, and finally a metal nano particle is added to react and combine with the second functional group. The core-shell metal nano photocatalyst composite material synthesized by the invention can effectively utilize visible light, and has the effects of decomposing formaldehyde, decomposing nitrogen oxides and inhibiting bacteria. In addition, the metal nano photocatalyst composite material of the present invention can improve the conversion efficiency of photovoltaic cells.
Description
Technical field
The present invention relates to a kind of composite, particularly a kind of hud typed (core shell) metal nanometer photocatalyst compound material and manufacture method thereof.
Background technology
Catalyst is a kind of chemical substance, and itself can reduce chemical reaction energy needed (activation energy) and promote the generation of chemical reaction or the speed of accelerated reaction, but itself does not change.
Photochemical catalyst then is to utilize the energy of specific wavelength light source to produce the effect of catalysis under light source irradiation, the extremely strong free radical of these oxidizing forces almost can decompose all to human body or the harmful organic substance of environment, and oxygen around making and molecular excitation become to have active OH and O
2Free radical can produce sterilization, suppress effects such as virus, deodorizing, decomposing organic matter.
Titanium dioxide (Titanium Dioxide, TiO
2) because have powerful redox ability, chemically stability height and nontoxic characteristic, be often used as material peace and quiet or experiment most.Titanium dioxide itself has two kinds of more common crystal structures, be respectively rutile mutually and anatase mutually, and the titanium dioxide of anatase phase has better photocatalyst activity, so the research of most photochemical catalyst all is conceived to this.After titanium dioxide optical catalyst was subjected to greater than the irradiation of the light of titanium dioxide band gap width, electronics can transit to conduction band from valence band, thereby produced electron-hole pair.Electronics tool reproducibility wherein, hole tool oxidisability, the hole can and titanium dioxide surface on the OH-reaction generate the very high OH-free radical of oxidisability, electronics then can with oxygen molecule in conjunction with formation superoxide ion (O
2-), active OH-free radical and superoxide ion can decompose organic matter, become carbon dioxide and water, thereby reach clean-up effect.
Aspect light source, because the band-gap energy size of anatase phase titanium dioxide is about 3.2 electron-volts, being equivalent to wavelength is the entrained energy of light wave of 387.5 nanometers (nm), so desire with the electronics of titanium dioxide from valence to conduction band, the ultraviolet light source of wavelength less than 387.5 nanometers must be provided, just can make titanium dioxide produce the photochemical catalyst reaction.Because the character of the decomposing organic matter of titanium dioxide optical catalyst and Superhydrophilic, so have antibiotic, antifouling, demist, deodorization, water purification, six big functions such as anticancer.Because many-sided application claims that in Japan photochemical catalyst is " a dreamlike material ".Because titanium dioxide optical catalyst is employed to be the light source of ultraviolet light wave band, again because the ultraviolet light energy in the daylight only to account for gross energy about 5%, make the range of application of titanium dioxide optical catalyst be very restricted.The energy of the sunlight medium ultraviolet light of fine open air has four milliwatts approximately, enough photochemical catalyst decomposing pollutant matter.But indoor fluorescent lamp has only 0.1～1 microwatt (μ W), and is for most photochemical catalyst, all not enough so that its generation effect.Therefore desire uses the titanium dioxide optical catalyst that utilizes the ultraviolet light reaction to carry out indoor air quietness, function such as antibiotic at home, all depends on the lifting of optically catalytic TiO 2 efficient.
In sum, exploitation one possesses the high response type photochemical catalyst of ultraviolet light and visible absorption wave band simultaneously, in the hope of being widely used in the people's livelihood purposes, is one of direction of relevant dealer's effort always.Demand at visible-light photocatalyst, also there are some photochemical catalysts to carry out ion modification, make the absorption region of its energy rank, yet this kind ion modification photochemical catalyst is nothing more than implanting transition metal ion (Cr, V, Ag) and nonmetallic ion (C, N, H) etc. between visible light.The photochemical catalyst that this type of ion injects has more unsettled energy scalariform condition at the point that injects mostly, and therefore the reaction to visible light is not very stable, tends to make its visible light catalytic ability that the phenomenon that weakens be arranged along with the growth of time.
Summary of the invention
Main purpose of the present invention is to be desirable to provide a hud typed metal nanometer photocatalyst compound material, all can react to have concurrently simultaneously at ultraviolet light and visible light wave range.
Another main purpose of the present invention is the method that is desirable to provide a kind of manufacturing hud typed (coreshell) metal nanometer photocatalyst compound material, to produce the metal nanometer photocatalyst compound material that can be simultaneously reacts at ultraviolet light and visible light wave range.
For reaching above-mentioned purpose, the invention provides a kind of method of manufacturing hud typed (core shell) metal nanometer photocatalyst compound material, this method comprises: the titanium dioxide (TiO that at first forms a nanometer particle size
2) particle solution, then in this solution, add the polyfunctional compound that has first functional group and second functional group simultaneously, this TiO 2 particles is to join by the reaction of this first functional group and this polyfunctional compound, adds a metal nanoparticle at last and reacts with this second functional group and combine.
In addition, the present invention also provides a kind of hud typed metal nanometer photocatalyst compound material, and it comprises:
One core is metal nanoparticle;
One nucleocapsid is titanium dioxide nano-particle.
The hud typed metal nanometer photocatalyst compound material that the present invention synthesized can effectively utilize visible light, and has decomposing formaldehyde, decomposing nitrogen oxide and antibacterial effect.In addition, metal nanometer photocatalyst compound material of the present invention can promote photronic conversion efficiency.
Description of drawings
By following detailed description in conjunction with the accompanying drawings, the plurality of advantages of can come into plain view summary of the invention and the present invention, wherein:
Fig. 1 is the present invention disclosed hud typed (core shell) metal nanometer photocatalyst compound material structural representation.
Fig. 2 A is the synthetic metal nanometer photocatalyst compound material schematic diagram of a preferred embodiment of the present invention.
Fig. 2 B is the abosrption spectrogram of gold nano photocatalyst compound material among Fig. 2 A.
Fig. 3 A is the synthetic metal nanometer photocatalyst compound material schematic diagram of another preferred embodiment of the present invention.
Fig. 3 B is the abosrption spectrogram of silver-colored nanometer photocatalyst compound material among Fig. 3 A.
Fig. 4 is methyl blue decolorization experiment figure as a result.
Fig. 5 is formaldehyde decomposition run testing result figure.
Fig. 6 is decompose nitrogen oxides result of the test figure.
Fig. 7 A utilizes gold nano photocatalyst compound material of the present invention to carry out the result of the antibacterial test of gram-positive bacteria.
Fig. 7 B utilizes gold nano photocatalyst compound material of the present invention to carry out the result of the antibacterial test of Gram-negative bacteria.
Fig. 8 is the photoelectric material test result.
The specific embodiment
Disclosed is a kind of hud typed (core shell) metal nanometer photocatalyst compound material, wishes to utilize the surface electrical photoresonance effect of metal nanoparticle so that the utilize ability of photochemical catalyst to the sunshine except the ultraviolet light wave band to be provided.In order to make narration of the present invention more detailed and complete, enumerate two preferred embodiments with explanation the present invention.Please refer to following description and cooperate following graphic.
Disclosed hud typed (core shell) metal nanometer photocatalyst compound material is meant that the metallic with a kind of nanometer particle size is a nuclear, and forms the formed composite of shell with TiO 2 particles growth outside nuclear of nanometer particle size.Please refer to Fig. 1, Fig. 1 is the present invention disclosed hud typed (core shell) metal nanometer photocatalyst compound material structural representation.The composite of common two kinds of formation that material mixes (for example alloy) can represent new physics, chemical property.And hud typed composite under the proper situation of control, then can be possessed the unique property of two kinds of materials.The present invention then be wish to see through the stratum nucleare metal nanoparticle in the absorption of visible light wave range to improve the photochemical catalyst utilization ratio of shell titanium dioxide.
The present invention also discloses a kind of manufacture method of manufacturing hud typed (core shell) metal nanometer photocatalyst compound material: the titanium dioxide (TiO that at first forms nanometer particle size (particle size distribution is between 0.1～200nm)
2) particle solution, then in this solution, adding the polyfunctional compound that has first functional group and second functional group simultaneously, this moment, TiO 2 particles joined by first functional group and polyfunctional compound reaction.Next add metal nanoparticle, this metal nanoparticle and second functional group carry out reaction bonded to form metal nanometer photocatalyst compound material of the present invention by covalent bond, are a core by metal nanoparticle is formed and nucleocapsid is made up of TiO 2 particles structure.
The first wherein above-mentioned functional group can be aliphatic or aromatic series functional group.And second functional group can be aliphatic or aromatic series functional group.In following preferred embodiment, we use the polyfunctional compound of siliceous oxyalkyl of a while and sulfydryl in composite synthetic reaction of the present invention.
Please refer to Fig. 2 A, be the synthetic metal nanometer photocatalyst compound material schematic diagram of a preferred embodiment of the present invention.The core of the metal nanometer photocatalyst compound material among Fig. 2 A is made up of a golden nanometer particle.At first utilize Ti (OH)
4Carrying out hot reflux (90 ℃) grew tiny TiO 2 particles in about two hours (particle size distribution is after 1～200nm), add polyfunctional compound with siloxanes and sulfydryl, make and titanium dioxide surface and this siloxanes-sulfydryl polyfunctional compound reaction finally connect Si-R at titanium dioxide surface
2-SH adds golden nanometer particle at last again, makes itself and sulfydryl with covalent bonds, finally obtains hud typed composite construction as shown in FIG..
Particularly, with 10%Ti (OH)
4Aqueous solution 3l carry out hot reflux 2 hours at 90 ℃, grown particle size distribution behind the TiO 2 particles of 1～200nm, add γ-mercaptopropyl trimethoxysilane ((CH of 10ml 10%
3O)
3-Si-(CH)
3-SH) ethanol solution continues to carry out hot reflux 1.5 hours, makes titanium dioxide surface and γ-mercaptopropyl trimethoxysilane reaction finally to connect Si-(CH) at titanium dioxide surface
3-SH, the last aqueous solution 1l that adds the 300ppm golden nanometer particle again makes itself and sulfydryl with covalent bonds, refluxes about 8 hours at 90 ℃, makes titanic oxide material be coated golden nanometer particle, and then obtains hud typed composite construction of the present invention.
In order to illustrate that resultant metal nanometer photocatalyst compound material of the present invention has the function of the sunshine of utilization except ultraviolet light, we carry out the spectral absorption test to above-mentioned gold nano photocatalyst compound material, please refer to Fig. 2 B, is its abosrption spectrogram.Curve 1 among Fig. 2 B is the abosrption spectrogram when only titanium dioxide optical catalyst being arranged, and curve 2 is the abosrption spectrogram of gold nano photocatalyst compound material.Can find out that curve 1 only has absorption at ultraviolet light wave band (380nm), the compound curve 2 of going up gold nano then tangible absorption also occurs at visible region.Therefore be obviously visible for the evidence that can utilize Different Light.
Nanosecond science and technology prosperity at present, except golden nanometer particle, other metal nanoparticle also can stably be synthesized out, the present invention does not also limit employed metal nanoparticle material, the visual different light environment of operator is served as the core of composite of the present invention to select suitable metal nanoparticle, to carry out the absorption of energy.Please refer to Fig. 3 A, be the synthetic metal nanometer photocatalyst compound material schematic diagram of another preferred embodiment of the present invention.The core of the metal nanometer photocatalyst compound material among Fig. 3 A is made up of Nano silver grain.Be same as above-mentioned gold nano photocatalyst compound material, also be to use one to contain the polyfunctional compound of sulfydryl and silicone functionalities simultaneously among Fig. 3 A as the polyfunctional compound in the building-up process.Other please refer to Fig. 3 B, is the abosrption spectrogram of above-mentioned silver-colored nanometer photocatalyst compound material.Curve 1 is the abosrption spectrogram when only titanium dioxide optical catalyst being arranged, and curve 2 is the abosrption spectrogram of silver-colored nanometer photocatalyst compound material.Can find out that by the distribution of two curves silver-colored nanometer photocatalyst compound material has bigger light abstraction width when similarly more only titanium dioxide optical catalyst being arranged.
In addition, traditional titanium dioxide optical catalyst also has methyl blue (Methyleneblue) characteristics of decolouring easily that make, we are also at these characteristics, as sample, detect whether still have this function with above-mentioned gold nano photocatalyst compound material and silver-colored nanometer photocatalyst compound material.Please refer to Fig. 4, is methyl blue decolorization experiment figure as a result.
Can find out by the experimental result broken line among Fig. 4, compared to the titanium dioxide optical catalyst that only is exposed under the ultraviolet light, employed two embodiment in this experiment (gold or silver) all have preferable methyl blue decolorizing efficiency, have confirmed that again the hud typed metal nanometer photocatalyst compound material that the present invention synthesized has the function that can effectively utilize visible light really.
Except decolouring test, titanium dioxide optical catalyst also possesses to have and purifies air and antibacterial effect.Carry out decomposing formaldehyde, decomposing nitrogen oxide and antibacterial test with the gold nano photocatalyst compound material again with next.
Please refer to Fig. 5, is formaldehyde decomposition run testing result figure.This method is the method for testing according to Japanese ISR1701-1, is continuing to feed under the condition of formaldehyde, uses the gold nano photocatalyst compound material as sample, measures formaldehyde removal amount in five hours.Can see that concentration of formaldehyde is along with the variation of time among Fig. 5, in the time section that visible light source is opened, the gold nano photocatalyst compound material has the effect that absorbs visible light and decomposing formaldehyde really.
Please refer to Fig. 6, is decompose nitrogen oxides result of the test figure.This method is the method for testing according to Japanese JISC TRZ0018, uses the gold nano photocatalyst compound material as sample, is tiled on the culture dish will testing powder on the circular reactor, and to carry out the test of decomposing nitrogen oxide, test condition is as shown in table 1 below.In five hours testing time, in the test powder of 0.9934 gram, removed the nitric oxide (NO) of 3.24 μ mol, produced the nitrogen dioxide of 2.09 μ mol, so total removal amount of nitrogen oxide (NOx) is 1.15 μ mol.Prove again that promptly metal nanometer photocatalyst compound material of the present invention does not lose titanium dioxide optical catalyst function originally.
Table 1
| Test condition | Numerical value |
| NO concentration | 1ppm |
| The test gas flow | 1l/min |
| Light radiation illumination | 1.5mW/cm 2 |
| Temperature | 25℃ |
| Relative humidity | 65％ |
| The |
5 hours |
Please refer to Fig. 7 A～Fig. 7 B, is to utilize gold nano photocatalyst compound material of the present invention to carry out the table as a result of antibacterial test.Among Fig. 7 A the bacterial strain that uses be staphylococcus aureus (gram-positive bacteria), employed bacterial strain is Escherichia coli (Gram-negative bacterias) among Fig. 7 B.After the fluorescent tube with wavelength 543nm shines 24 hours as light source, can see that the result who has added gold nano photocatalyst compound material of the present invention is: no matter be gram-positive bacteria or negative bacterium, clump count is all less than 10 CFU (colonyforming units).
Energy demand in recent years constantly increases, but the available energy (for example oil) will be soon depleted in the end of the century again.The human energy source that can replace fossil fuel of always seeking; And from sunshine continuously, obtain required energy, be main research direction always.The replacement scheme that is suggested comprises various photoelectrochemical cells (photoelectrochemical cell), though cost is lower, never as high conversion efficiency as the solid state solar cell, thereby also can't replace.Titanium dioxide in the dyestuff photocell of a kind of new architecture that is suggested in recent years, also is used to the role who serves as anode except as the photochemical catalyst.The metal nano catalyst material that we also attempt that the present invention is synthesized is applied on this type of photocell and (is sprayed on its anode), and by testing open circuit voltage and the open-circuit current that can represent photocell efficient, detects its efficient.Please refer to Fig. 8, is the photoelectric material table with test results.Can find that its open circuit voltage of the photocell of metal nanometer photocatalyst compound material of the present invention and open-circuit current all have the trend of obvious rising in the spraying, have an opportunity really to promote photronic conversion efficiency by the table results among Fig. 8.
The above only is preferred embodiment of the present invention; so it is not in order to limit scope of the present invention; any those of ordinary skill in the art; without departing from the spirit and scope of the present invention; can do further improvement and variation on this basis, so the scope that claims were defined that protection scope of the present invention is worked as with the application is as the criterion.
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| CN103933972A (en) * | 2014-04-21 | 2014-07-23 | 国家纳米科学中心 | Method for preparing precious metal titanium dioxide core-shell structure |
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| WO2000044507A1 (en) * | 1999-01-28 | 2000-08-03 | The Board Of Regents For Oklahoma State University | Thin films of core-shell nanoparticles |
| CN1142014C (en) * | 2002-11-12 | 2004-03-17 | 中国地质大学（武汉） | Method for supporting titanium dioxide photocatalyst on metal surface |
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| CN103933972A (en) * | 2014-04-21 | 2014-07-23 | 国家纳米科学中心 | Method for preparing precious metal titanium dioxide core-shell structure |
| CN104001506B (en) * | 2014-06-10 | 2016-04-13 | 天津大学 | A kind of alcohols photooxidation catalyst and its preparation method and application |
| CN104492432A (en) * | 2014-12-13 | 2015-04-08 | 济南大学 | Hollow bimetal nanoparticle/titanium dioxide core-shell structure, and preparation method and application thereof |
| CN104492432B (en) * | 2014-12-13 | 2017-07-04 | 济南大学 | Hollow bimetal nano particles/titanium dioxide core shell structure and its preparation method and application |
| CN107096531A (en) * | 2016-02-22 | 2017-08-29 | 天津大学 | Gold-titanium dioxide core-shell structure photochemical catalyst of noble metal gold modification and preparation method thereof |
| CN113731387A (en) * | 2020-05-28 | 2021-12-03 | 长春理工大学 | Cheap metal/semiconductor composite photocatalyst for treating organic pollutants in water and preparation method thereof |
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